CN103819210B - Method for preparing Ca-Mg functional material through in-situ decomposition reaction - Google Patents
Method for preparing Ca-Mg functional material through in-situ decomposition reaction Download PDFInfo
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- CN103819210B CN103819210B CN201410004538.XA CN201410004538A CN103819210B CN 103819210 B CN103819210 B CN 103819210B CN 201410004538 A CN201410004538 A CN 201410004538A CN 103819210 B CN103819210 B CN 103819210B
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- functional materials
- hydrotalcite
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Abstract
The invention relates to a method for preparing a Ca-Mg functional material through an in-situ decomposition reaction. The method comprises the technical scheme as follows: mixing 30-60 wt% of magnesia particles, 10-30 wt% of magnesia powder, 5-40 wt% of limestone, 5-15 wt% of Mg-Al hydrotalcite, 0-10 wt% of water and 0-4 wt% of a bonding agent, uniformly stirring, and molding; drying molded blank at a temperature of 110 DEG C for 4-24 hours, keeping at the temperature of 200-1100 DEG C for 1-8 hours, and obtaining the Ca-Mg functional material. The method provided by the invention has the advantages that the process is simple and raw materials are rich. The prepared Ca-Mg functional material has small volume density, excellent heat preservation and insulation performance, high strength, excellent erosion resistance, good volume stability at high temperature, excellent thermal shock resistance, good molten steel purifying effect, rich raw material, simplicity in construction and wide application range.
Description
Technical field
The invention belongs to the calcareous technical field of function materials of magnesium, particularly relate to the method that the calcareous functional materials of magnesium is prepared in the reaction of a kind of decomposition in situ.
Background technology
Along with the growing tension of the energy, various countries are to the development of hot industry energy-saving material, production and use pay attention to day by day.Lightweight and half lightweight refractory due to light weight, void content is high, volume density is little and thermal conductivity is low, with the obvious advantage energy-conservation, is thus widely applied at hot industry, serves insulation and energy-saving and cost-reducing effect.
The main chemical compositions of existing lightweight and half lightweight refractory is aluminum oxide and silicon-dioxide, belongs to traditional aluminium silicon based material, and the essential mineral of material is that corundum, mullite, quartz and glass are equal.Because aluminium silicon system refractory raw material is laid in abundant on earth, thus in the application in heat preserving and insulating material field, occupy dominant position always.But, aluminium silicon system lightweight refractory belongs to acid or amphoteric refractory, be only applicable to acid and neutral Working environment, it is in applied at elevated temperature process, alkaline matter easily and in environment or material react, cause the generation of low melt-phase, mechanical property and the work-ing life of light material can be had a strong impact on.Thus, alkaline light material is developed to become one of focal point to the needs of insulation and lagging material in satisfied alkaline environment for use.At present, research, the Synthesis and applications of alkaline light material have been reported, wherein:
The main ingredient of material is periclasite and a magnesium-aluminium spinel, can reach the object used in alkaline environment.Its preparation method is: by magnesite powder, light-magnesite powder, alumine powder, aluminium hydrate powder and can burn lost article mixing, external adding water and bonding agent stir, through shaping, dry, burn till, be incubated and cool after obtain.Though such synthetic method has its advantage, as: the main mine phase periclasite of material and the fire performance of magnesium-aluminium spinel excellent, alkali-resistivity matter corrodes ability is strong, but the shortcoming existed also is obvious, namely the technics comparing preparing lightweight periclasite-fireproof magnesia alumina spinel material is complicated, raw material type is more, and mixing time is long, higher to the performance requriements of mixing equipment.Simultaneously, the mode of mechanically mixing is adopted to be difficult to make various feed distribution even, the carrying out of correlated response in compound is also insufficient, after high temperature burns till, be difficult to obtain microstructure and the uniform light material of chemical composition, do not reach the original intention of material designer, thus cause the physicals of material unstable, insulation and effect of heat insulation are difficult to meet hot industry needs.
Another kind of alkaline light material is the use of the magnesium calcareous material of Wingdale, and main ingredient is periclasite, calcium magnesia sand and square calcium stone.Its method prepared is: by magnesia and Wingdale (calcium carbonate) mixing, add organic or inorganic bonding agent simultaneously, undertaken making lining by the method for dry type vibratory or spraying.The advantage of this synthetic materials has well clean effect to molten steel, can adsorb the oxide inclusion in steel and sulphur and phosphorus etc.Shortcoming is that the limestone particle size owing to using is comparatively large, and the hot strength of material can be caused after Wingdale at high temperature decomposes to reduce, molten steel infiltration aggravation in the material.
Summary of the invention
The present invention is intended to overcome prior art defect, and object is to provide the method that the calcareous functional materials of magnesium is prepared in the decomposition in situ reaction that is simple and abundant raw materials of a kind of technique; The magnesium prepared by the method calcareous functional materials volume density is little, heat preservation and insulation is excellent, intensity is high, erosion-resisting characteristics is excellent, high volume good stability, thermal shock resistance can excellent, purify hot metal is effective, easy construction and use range wide.
For achieving the above object, the technical solution used in the present invention is: first mixed by the bonding agent of the magnesium aluminum-hydrotalcite of the Wingdale of the magnesia powder of the magnesia particle of 30 ~ 60wt%, 10 ~ 30wt%, 5 ~ 40wt%, 5 ~ 15wt%, the water of 0 ~ 10wt% and 0 ~ 4wt%, stir, shaping; Again by the base substrate after shaping under 110 DEG C of conditions dry 4 ~ 24 hours, then under 200 ~ 1100 DEG C of conditions, be incubated 1 ~ 8 hour, obtain the calcareous functional materials of magnesium.
Content of MgO >=95wt% in described magnesia particle; The particle diameter of magnesia particle is 0.2 ~ 11mm.
Content of MgO >=95wt% in described magnesia powder; The particle diameter of magnesia powder is 3 ~ 200 μm.
CaCO in described Wingdale
3content>=90wt%; Particle diameter≤the 100nm of Wingdale.
Mg in described magnesium aluminum-hydrotalcite
(4-6)al
2(OH)
(12-16)(CO
3) 4H
2o content>=90wt%, the granularity≤0.2mm of magnesium aluminum-hydrotalcite.
Described forming method is the shaping or casting of dry type vibratory.
Described bonding agent is dextrin or is polyvinyl alcohol, uses during described bonding agent casting.
Owing to adopting technique scheme, the present invention compared with prior art has following positively effect:
The present invention is by adding nanometer Wingdale, and at high temperature generate active very high calcium oxide, play the effect of purify hot metal, owing to using nanometer Wingdale, the air vent aperture that its decomposition reaction is formed is very little, obviously can not reduce the intensity of material; The reaction of magnesium aluminum-hydrotalcite decomposition in situ forms periclasite-magnesium-aluminium spinel mixed binding system in material, is evenly distributed in by granular cementation in matrix of materials, improves the middle hot strength of material.The problem that product prepared by the present invention can avoid prior art to cause structure and component inequality because adopting multiple starting material to mix and then react the light material prepared.
Typical magnesium aluminum-hydrotalcite Mg
6al
2(OH)
16(CO
3) 4H
2o is a kind of naturally occurring mineral, is widely used in fields such as catalyzer, medicine, makeup, coating and plastic workings.The store content of occurring in nature magnesium aluminum-hydrotalcite is limited, and thus people prepare magnesium aluminum-hydrotalcite by the method for various synthesis, and primary synthetic methods comprises: coprecipitation method, ion exchange method, roast reduction process etc.In the building-up process of magnesium aluminum-hydrotalcite, due to the difference of technology controlling and process and batching, there is certain difference in the synthetic magnesium aluminum-hydrotalcite obtained, be embodied in Mg in chemical composition
2+and OH
-in the difference of amount of ions, its general formula can use Mg
(4-6)al
2(OH)
(12-16)(CO
3) 4H
2o represents.Hydrotalcite starts to decompose at 200 DEG C ~ about 250 DEG C, and degradation production can play the effect of consolidating material particle, and the bonding agent that can be used as material when adopting dry type vibratory shaping uses.
After Wingdale in the present invention and magnesium aluminum-hydrotalcite decompose, discharge carbonic acid gas and water vapor, leave micropore in position, the mineral composition of material is the high temperature ore deposit phases such as periclasite, square calcium stone (calcium oxide) and magnesium-aluminium spinel.
The production method of the relatively existing synthetic insulating material of the present invention, preparation technology is simple, can obtain the magnesium calcareous material of uniform texture; Relative to existing magnesium calcareous material, the feature that prepared matrix material has that volume density is less, intensity is higher, erosion-resisting characteristics is excellent, high volume good stability and thermal shock resistance can be excellent.Meanwhile, owing to employing nano-calcium carbonate, the strength of materials is higher than traditional MgO-CaO refractory, and the ability of purify hot metal is also stronger.The inner lining material of the kiln and container that can be used as pyrometallurgy industry uses.Therefore the present invention can obtain component and even structure take into account the heat insulation and calcareous functional materials of magnesium that is purify hot metal effect.
Therefore, simple and the abundant raw materials of present invention process, prepared magnesium calcareous functional materials volume density is little, heat preservation and insulation is excellent, intensity is high, erosion-resisting characteristics is excellent, high volume good stability and thermal shock resistance can excellent, purify hot metal is effective, abundant raw materials, easy construction and use range are wide.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, the restriction not to its protection domain.
In this embodiment: the content of MgO>=95wt% in described magnesia particle; The particle diameter of magnesia particle is 0.2 ~ 11mm; Content of MgO>=95wt% in described magnesia powder; The particle diameter of magnesia powder is 3 ~ 200 μm; CaCO in described Wingdale
3content>=90wt%; Particle diameter≤the 100nm of Wingdale; Mg in described magnesium aluminum-hydrotalcite
(4-6)al
2(OH)
(12-16)(CO
3) 4H
2o content>=90wt%, the granularity≤0.2mm of magnesium aluminum-hydrotalcite.Described bonding agent is dextrin or is polyvinyl alcohol, uses during described bonding agent casting.Repeat no more in embodiment.
embodiment 1
The method of the calcareous functional materials of magnesium is prepared in a kind of decomposition in situ reaction.First the bonding agent of the magnesium aluminum-hydrotalcite of the Wingdale of the magnesia powder of the magnesia particle of 40 ~ 60wt%, 10 ~ 25wt%, 5 ~ 15wt%, 10 ~ 15wt%, the water of 1 ~ 5wt% and 1 ~ 2wt% is mixed, stir, casting; Again by the base substrate after shaping under 110 DEG C of conditions dry 4 ~ 12 hours, then under 200 ~ 500 DEG C of conditions, be incubated 1 ~ 4 hour, obtain the calcareous functional materials of magnesium.
embodiment 2
The method of the calcareous functional materials of magnesium is prepared in a kind of decomposition in situ reaction.First the water of the magnesium aluminum-hydrotalcite of the Wingdale of the magnesia powder of the magnesia particle of 40 ~ 60wt%, 10 ~ 25wt%, 5 ~ 15wt%, 10 ~ 15wt%, 1 ~ 5wt% is mixed, stir, casting; Again by the base substrate after shaping under 110 DEG C of conditions dry 4 ~ 12 hours, then under 500 ~ 700 DEG C of conditions, be incubated 1 ~ 4 hour, obtain the calcareous functional materials of magnesium.
embodiment 3
The method of the calcareous functional materials of magnesium is prepared in a kind of decomposition in situ reaction.First the bonding agent of the Wingdale of the magnesia powder of the magnesia particle of 40 ~ 60wt%, 10 ~ 25wt%, 5 ~ 20wt%, the magnesium aluminum-hydrotalcite of 10 ~ 15wt% and 2 ~ 4wt% is mixed, stir, casting; Again by the base substrate after shaping under 110 DEG C of conditions dry 4 ~ 12 hours, then under 300 ~ 400 DEG C of conditions, be incubated 5 ~ 8 hours, obtain the calcareous functional materials of magnesium.
embodiment 4
The method of the calcareous functional materials of magnesium is prepared in a kind of decomposition in situ reaction.First the bonding agent of the magnesium aluminum-hydrotalcite of the Wingdale of the magnesia powder of the magnesia particle of 40 ~ 60wt%, 10 ~ 25wt%, 15 ~ 30wt%, 5 ~ 10wt%, the water of 6 ~ 10wt% and 3 ~ 4wt% is mixed, stir, casting; Again by the base substrate after shaping under 110 DEG C of conditions dry 13 ~ 24 hours, then under 600 ~ 1100 DEG C of conditions, be incubated 5 ~ 8 hours, obtain the calcareous functional materials of magnesium.
embodiment 5
The method of the calcareous functional materials of magnesium is prepared in a kind of decomposition in situ reaction.First mixed by the magnesium aluminum-hydrotalcite of the magnesia powder of the magnesia particle of 40 ~ 60wt%, 10 ~ 25wt%, the Wingdale of 15 ~ 30wt% and 10 ~ 15wt%, stir, dry type vibratory is shaping; Again by the base substrate after shaping under 110 DEG C of conditions dry 4 ~ 10 hours, then under 200 ~ 500 DEG C of conditions, be incubated 1 ~ 4 hour, obtain the calcareous functional materials of magnesium.
embodiment 6
The method of the calcareous functional materials of magnesium is prepared in a kind of decomposition in situ reaction.First mixed by the magnesium aluminum-hydrotalcite of the magnesia powder of the magnesia particle of 40 ~ 50wt%, 10 ~ 25wt%, the Wingdale of 30 ~ 40wt% and 5 ~ 10wt%, stir, dry type vibratory is shaping; Again by the base substrate after shaping under 110 DEG C of conditions dry 11 ~ 16 hours, then under 600 ~ 1100 DEG C of conditions, be incubated 5 ~ 8 hours, obtain the calcareous functional materials of magnesium.
embodiment 7
The method of the calcareous functional materials of magnesium is prepared in a kind of decomposition in situ reaction.First mixed by the magnesium aluminum-hydrotalcite of the magnesia powder of the magnesia particle of 30 ~ 55wt%, 20 ~ 30wt%, the Wingdale of 20 ~ 30wt% and 5 ~ 10wt%, stir, dry type vibratory is shaping; Again by the base substrate after shaping under 110 DEG C of conditions dry 17 ~ 24 hours, then under 500 ~ 1100 DEG C of conditions, be incubated 3 ~ 5 hours, obtain the calcareous functional materials of a kind of magnesium.
This embodiment compared with prior art has following positively effect:
This embodiment is by adding nanometer Wingdale, and at high temperature generate active very high calcium oxide, play the effect of purify hot metal, owing to using nanometer Wingdale, the air vent aperture that its decomposition reaction is formed is very little, obviously can not reduce the intensity of material; The reaction of magnesium aluminum-hydrotalcite decomposition in situ forms periclasite-magnesium-aluminium spinel mixed binding system in material, is evenly distributed in by granular cementation in matrix of materials, improves the middle hot strength of material.The problem that product prepared by this embodiment can avoid prior art to cause structure and component inequality because adopting multiple starting material to mix and then react the light material prepared.
Typical magnesium aluminum-hydrotalcite Mg
6al
2(OH)
16(CO
3) 4H
2o is a kind of naturally occurring mineral, is widely used in fields such as catalyzer, medicine, makeup, coating and plastic workings.The store content of occurring in nature magnesium aluminum-hydrotalcite is limited, and thus people prepare magnesium aluminum-hydrotalcite by the method for various synthesis, and primary synthetic methods comprises: coprecipitation method, ion exchange method, roast reduction process etc.In the building-up process of magnesium aluminum-hydrotalcite, due to the difference of technology controlling and process and batching, there is certain difference in the synthetic magnesium aluminum-hydrotalcite obtained, be embodied in Mg in chemical composition
2+and OH
-in the difference of amount of ions, its general formula can use Mg
(4-6)al
2(OH)
(12-16)(CO
3) 4H
2o represents.Hydrotalcite starts to decompose at 200 DEG C ~ about 250 DEG C, and degradation production can play the effect of consolidating material particle, and the bonding agent that can be used as material when adopting dry type vibratory shaping uses.
After Wingdale in this embodiment and magnesium aluminum-hydrotalcite decompose, discharge carbonic acid gas and water vapor, leave micropore in position, the mineral composition of material is the high temperature ore deposit phases such as periclasite, square calcium stone (calcium oxide) and magnesium-aluminium spinel.
The production method of the relatively existing synthetic insulating material of this embodiment, preparation technology is simple, can obtain the magnesium calcareous material of uniform texture; Relative to existing magnesium calcareous material, the feature that prepared matrix material has that volume density is less, intensity is higher, erosion-resisting characteristics is excellent, high volume good stability and thermal shock resistance can be excellent.Meanwhile, owing to employing nano-calcium carbonate, the strength of materials is higher than traditional MgO-CaO refractory, and the ability of purify hot metal is also stronger.The inner lining material of the kiln and container that can be used as pyrometallurgy industry uses.Therefore this embodiment can obtain component and even structure take into account the heat insulation and calcareous functional materials of magnesium that is purify hot metal effect.
Therefore, simple and the abundant raw materials of this embodiment technique, prepared magnesium calcareous functional materials volume density is little, heat preservation and insulation is excellent, intensity is high, erosion-resisting characteristics is excellent, high volume good stability and thermal shock resistance can excellent, purify hot metal is effective, abundant raw materials, easy construction and use range are wide.
Claims (6)
1. a decomposition in situ reacts the method preparing the calcareous functional materials of magnesium, it is characterized in that first the bonding agent of the magnesium aluminum-hydrotalcite of the Wingdale of the magnesia powder of the magnesia particle of 30 ~ 60wt%, 10 ~ 30wt%, 5 ~ 40wt%, 5 ~ 15wt%, the water of 0 ~ 10wt% and 0 ~ 4wt% being mixed, stir, shaping; Again by the base substrate after shaping under 110 DEG C of conditions dry 4 ~ 24 hours, then under 200 ~ 1100 DEG C of conditions, be incubated 1 ~ 8 hour, obtain the calcareous functional materials of magnesium;
CaCO in described Wingdale
3content>=90wt%; Particle diameter≤the 100nm of Wingdale.
2. the method for the calcareous functional materials of magnesium is prepared in decomposition in situ reaction according to claim 1, it is characterized in that the content of MgO >=95wt% in described magnesia particle; The particle diameter of magnesia particle is 0.2 ~ 11mm.
3. the method for the calcareous functional materials of magnesium is prepared in decomposition in situ reaction according to claim 1, it is characterized in that the content of MgO >=95wt% in described magnesia powder; The particle diameter of magnesia powder is 3 ~ 200 μm.
4. the method for the calcareous functional materials of magnesium is prepared in decomposition in situ reaction according to claim 1, it is characterized in that the Mg in described magnesium aluminum-hydrotalcite
(4-6)al
2(OH)
(12-16)(CO
3) 4H
2o content>=90wt%, the granularity≤0.2mm of magnesium aluminum-hydrotalcite.
5. the method for the calcareous functional materials of magnesium is prepared in decomposition in situ reaction according to claim 1, it is characterized in that described bonding agent is dextrin or is polyvinyl alcohol.
6. the method for the calcareous functional materials of magnesium is prepared in decomposition in situ reaction according to claim 1, it is characterized in that described forming method is the shaping or casting of dry type vibratory.
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| CN105272273A (en) * | 2015-09-24 | 2016-01-27 | 焦作市金鑫恒拓高温材料有限公司 | Calcium magnesium carbon composite material and preparation method |
| 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 |
| CN106518113A (en) * | 2016-11-06 | 2017-03-22 | 金少平 | Continuous casting tundish paint with good purification function and preparation method thereof |
| CN107324819A (en) * | 2017-06-13 | 2017-11-07 | 长兴华悦耐火材料厂 | A kind of dry-type vibration material and preparation method thereof |
| CN109485389A (en) * | 2018-11-23 | 2019-03-19 | 辽宁科技大学 | A kind of micropore calcium magnesite and preparation method thereof |
| CN112851380A (en) * | 2021-02-24 | 2021-05-28 | 中国一冶集团有限公司 | Magnesium-calcium metallurgical furnace lid castable and preparation method thereof |
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| CN101328071A (en) * | 2008-07-31 | 2008-12-24 | 武汉科技大学 | Magnesia-calcia dry type working liner for tundish and preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101328071A (en) * | 2008-07-31 | 2008-12-24 | 武汉科技大学 | Magnesia-calcia dry type working liner for tundish and preparation thereof |
Non-Patent Citations (2)
| Title |
|---|
| Porous alumina-spinel ceramics for high temperature applications;Rafael Salomao et al.;《Ceramics International》;20110203;第37卷;第1393-1399页 * |
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