CN104788121A - Mullite lightweight refractory material and preparation method thereof - Google Patents
Mullite lightweight refractory material and preparation method thereof Download PDFInfo
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- CN104788121A CN104788121A CN201510186484.8A CN201510186484A CN104788121A CN 104788121 A CN104788121 A CN 104788121A CN 201510186484 A CN201510186484 A CN 201510186484A CN 104788121 A CN104788121 A CN 104788121A
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Abstract
The invention relates to a mullite lightweight refractory material and a preparation method of the mullite lightweight refractory material. The invention adopts the technical scheme that the method comprises the steps of preparing materials under a 40-55 DEG C water bath condition according to a mass ratio of an AC (azodicarbonamide) foaming agent to polyethylene glycol 400 to ammonium bicarbonate to water of 1:(2-5):(1-4):(80-120), stirring, preparing foaming liquid, preparing materials at a mass ratio of the foaming liquid to rho-Al2O3 to gangue powder of (50-60):(1-3):100, stirring, forming to prepare a formed mixture, putting the formed mixture in a vacuum freeze drier for freeze drying for 72-84h, preparing a dried formed mixture, putting the dried formed mixture in a resistance furnace, holding temperature at 1280-1400DEG C for 45-50min, naturally cooling with the furnace, and obtaining the mullite lightweight refractory material. The method has the characteristics of low cost, simple technology and high finished product rate, and the prepared mullite lightweight refractory material is low in volume density, high in cold crushing strength and low in heat conductivity coefficient.
Description
Technical field
The invention belongs to lightweight refractory technical field.Be specifically related to a kind of mullite light refractory material and preparation method thereof.
Background technology
Along with people are to the pay attention to day by day of resource and environment, each hot industry field is also more and more higher to energy-saving and cost-reducing requirement, and lightweight (insulation/heat insulation) the refractory materials energy-saving material that to be high temperature kiln, Thermal Equipment etc. indispensable.Therefore, excellent, the cheap lightweight refractory of selectivity is directly connected to the energy-saving and emission-reduction of hot industry, is conducive to the smooth running ensureing hot industry simultaneously.
Mullite (3Al
2o
32SiO
2, be abbreviated as A
3s
2) there is the characteristic that fusing point is high, physical strength is large, thermal expansivity is little and chemical stability is good, be desirable middle-and-high-ranking refractory materials; In addition, raw material (coal gangue/flyash/bauxitic clay/" the three stone "/commercial alumina+silicon powder etc.) source of preparing mullite refractory is abundanter, therefore can reduce the cost of development of mullite light refractory material.
At present, the method preparing mullite light refractory material mainly contains chemical method, burns mistake method and foaming etc.
Chemical method is adopted to prepare lightweight refractory, mainly form pore (as the hydrolysis of metal A l powder produces hydrogen) with chemical reaction, by controlling the formation, distribution etc. of chemical reaction rate and then adjustment pore, then shaping, dry, finally burn till obtained lightweight refractory.But the distribution of its foaming chemical speed of reaction and bubble is difficult to control, and then have impact on the performance of lightweight refractory.
Adopt to burn and lose legal system for lightweight refractory, lost article (as sawdust, starch, coke etc.) pore-creating is burnt mainly through adding, in refractory materials sintering process, hole is left after burning lost article perfect combustion, and then obtained lightweight refractory, as " a kind of novel light mullite brick and preparation method thereof " (201310171084.0) and " one high alumina coal gangue mullite synthesizing light weight fire resistant materials " (201410182327.5).But the formation of its hole and pore size depend on the add-on and size of burning lost article completely, and easily crack in the lightweight refractory of preparation, can reduce the intensity of lightweight refractory.
Adopt foaming to prepare lightweight refractory, form foam mainly through whipping agent (as AC, SDBS etc.), then to mix with refractory slurry, shaping.In conjunction with " foaming+dry " technique (Dong Tonglin etc. foaming prepares mullite lightweight refractory technical study. Wuhan University Of Technology's journal, 2009,32 (2); Wang Hua etc. foaming slip casting method mullite synthesizing lightweight refractory. Fire Science, 2013,22 (2)), in refractory materials, leave hole, finally burn till, obtained lightweight refractory.But prepared mud moisture content is higher, in baking oven inner drying process, along with a large amount of effusions of moisture, foam is easy to break and causes shaping lightweight refractory to cave in damage.
Generally speaking, adopt chemical method to lose legal system for lightweight refractory with burning, the physicals of goods is poor; And foaming almost all adopts the preparation technology of " foaming+dry ", on the one hand, the intensity of foam and stability (foam not easily breaks) are difficult to ensure; On the other hand, in follow-up lightweight refractory drying course, the effusion of moisture easily causes breaking of foam, and then causes damage to a certain degree to lightweight refractory, reduces the yield rate of lightweight refractory.
Summary of the invention
The present invention is intended to overcome prior art defect, object is to provide a kind of preparation method of with low cost, technique is simple and yield rate is high mullite light refractory material, and the volume density of the mullite light refractory material prepared by the method is low, cold crushing strength is large and thermal conductivity is little.
For achieving the above object, the concrete steps of preparation method of the present invention are:
The first step, under 40 ~ 55 DEG C of water bath condition, AC whipping agent, poly(oxyethylene glycol) 400, bicarbonate of ammonia and water are inserted in container, stir 15 ~ 20 minutes, obtained expanding foam solution.Wherein, AC whipping agent: poly(oxyethylene glycol) 400: bicarbonate of ammonia: the mass ratio of water is 1: (2 ~ 5): (1 ~ 4): (80 ~ 120).
Second step, by expanding foam solution, ρ-Al
2o
3stir 5 ~ 8 minutes with Coal gangue powder, add die for molding, the compound after obtained shaping.Wherein, expanding foam solution: ρ-Al
2o
3: the mass ratio of Coal gangue powder is (50 ~ 60): (1 ~ 3): 100.
3rd step, the compound after shaping is placed in vacuum freeze drier lyophilize 72 ~ 84 hours, obtained dried shaping compound.
4th step, dried shaping compound is placed in resistance furnace, under 1280 ~ 1400 DEG C of conditions, is incubated 45 ~ 50 minutes, with stove naturally cooling, obtains mullite light refractory material.
Described AC whipping agent is chemical pure, Cellmic C 121 content >=96wt%.
Described poly(oxyethylene glycol) 400 is analytical pure.
Described bicarbonate of ammonia is analytical pure.
Described ρ-Al
2o
3granularity≤0.1 μm of powder; Al
2o
3content>=99wt%.
Granularity≤40 μm of described Coal gangue powder; The main chemical compositions of coal gangue is: Al
2o
3content>=60wt%, SiO
2content>=25wt%, Fe
2o
3content≤2wt%, (K
2o+Na
2o) content≤0.5wt%.
The lyophilize temperature of described vacuum freeze drier is-40 ~-45 DEG C, and vacuum pressure is 0.05 ~ 0.1Pa.
Owing to adopting technique scheme, the present invention compared with prior art has the following advantages:
The present invention adopts industrial solid castoff resource---and coal gangue is starting raw material, prepared mullite light refractory material with low cost.
The present invention is without the need to special Preparation equipment and treatment technology, and save human resources, technical process is simple.
The present invention, with " foaming " combination " vacuum lyophilization " technology, has ensured the froth stability of mullite light refractory material, has improve the yield rate of mullite light refractory material.
Mullite light refractory material prepared by the present invention, after measured: yield rate is 98 ~ 99%; Volume density is 0.60 ~ 0.95gcm
-3; Cold crushing strength is 4.5 ~ 8.0MPa; Thermal conductivity is 0.18 ~ 0.25Wm
-1k
-1.
Therefore, the present invention has with low cost, that technique is simple and yield rate is high feature; Prepared mullite light refractory material volume density is low, cold crushing strength is large and thermal conductivity is little.
Embodiment
Below in conjunction with embodiment, the invention will be further described, the restriction not to its protection domain.
For avoiding repetition, first by as follows for the technical parameter Unify legislation involved by this embodiment, repeat no more in embodiment:
Described AC whipping agent is chemical pure, Cellmic C 121 content >=96wt%.
Described poly(oxyethylene glycol) 400 is analytical pure.
Described bicarbonate of ammonia is analytical pure.
Described ρ-Al
2o
3granularity≤0.1 μm of powder; Al
2o
3content>=99wt%.
Granularity≤40 μm of described Coal gangue powder; The main chemical compositions of described coal gangue is: Al
2o
3content>=60wt%, SiO
2content>=25wt%, Fe
2o
3content≤2wt%, (K
2o+Na
2o) content≤0.5wt%.
The lyophilize temperature of described vacuum freeze drier is-40 ~-45 DEG C, and vacuum pressure is 0.05 ~ 0.1Pa.
embodiment 1
A kind of mullite light refractory material and preparation method thereof.The concrete steps of described preparation method are:
The first step, under 40 ~ 50 DEG C of water bath condition, AC whipping agent, poly(oxyethylene glycol) 400, bicarbonate of ammonia and water are inserted in container, stir 15 ~ 20 minutes, obtained expanding foam solution.Wherein, AC whipping agent: poly(oxyethylene glycol) 400: bicarbonate of ammonia: the mass ratio of water is 1: (2 ~ 4): (1 ~ 3): (80 ~ 96).
Second step, by expanding foam solution, ρ-Al
2o
3stir 6 ~ 8 minutes with Coal gangue powder, add die for molding, the compound after obtained shaping.Wherein, expanding foam solution: ρ-Al
2o
3: the mass ratio of Coal gangue powder is (50 ~ 55): (1 ~ 2): 100.
3rd step, the compound after shaping is placed in vacuum freeze drier lyophilize 72 ~ 80 hours, obtained dried shaping compound.
4th step, dried shaping compound is placed in resistance furnace, under 1280 ~ 1350 DEG C of conditions, is incubated 45 ~ 50 minutes, with stove naturally cooling, obtains mullite light refractory material.
Mullite light refractory material prepared by the present embodiment, after measured: yield rate is 98.6 ~ 98.8%; Volume density is 0.60 ~ 0.75gcm
-3; Cold crushing strength is 4.5 ~ 6.0MPa; Thermal conductivity is 0.18 ~ 0.21Wm
-1k
-1.
embodiment 2
A kind of mullite light refractory material and preparation method thereof.The concrete steps of described preparation method are:
The first step, under 40 ~ 50 DEG C of water bath condition, AC whipping agent, poly(oxyethylene glycol) 400, bicarbonate of ammonia and water are inserted in container, stir 15 ~ 20 minutes, obtained expanding foam solution.Wherein, AC whipping agent: poly(oxyethylene glycol) 400: bicarbonate of ammonia: the mass ratio of water is 1: (2 ~ 4): (1 ~ 3): (88 ~ 104).
Second step, by expanding foam solution, ρ-Al
2o
3stir 6 ~ 8 minutes with Coal gangue powder, add die for molding, the compound after obtained shaping.Wherein, expanding foam solution: ρ-Al
2o
3: the mass ratio of Coal gangue powder is (50 ~ 55): (2 ~ 3): 100.
3rd step, the compound after shaping is placed in vacuum freeze drier lyophilize 72 ~ 80 hours, obtained dried shaping compound.
4th step, dried shaping compound is placed in resistance furnace, under 1280 ~ 1350 DEG C of conditions, is incubated 45 ~ 50 minutes, with stove naturally cooling, obtains mullite light refractory material.
Mullite light refractory material prepared by the present embodiment, after measured: yield rate is 98.6 ~ 99.0%; Volume density is 0.65 ~ 0.70gcm
-3; Cold crushing strength is 5.0 ~ 5.5MPa; Thermal conductivity is 0.19 ~ 0.20Wm
-1k
-1.
embodiment 3
A kind of mullite light refractory material and preparation method thereof.The concrete steps of described preparation method are:
The first step, under 40 ~ 50 DEG C of water bath condition, AC whipping agent, poly(oxyethylene glycol) 400, bicarbonate of ammonia and water are inserted in container, stir 15 ~ 20 minutes, obtained expanding foam solution.Wherein, AC whipping agent: poly(oxyethylene glycol) 400: bicarbonate of ammonia: the mass ratio of water is 1: (2 ~ 4): (2 ~ 4): (96 ~ 112).
Second step, by expanding foam solution, ρ-Al
2o
3stir 6 ~ 8 minutes with Coal gangue powder, add die for molding, the compound after obtained shaping.Wherein, expanding foam solution: ρ-Al
2o
3: the mass ratio of Coal gangue powder is (55 ~ 60): (1 ~ 2): 100.
3rd step, the compound after shaping is placed in vacuum freeze drier lyophilize 76 ~ 84 hours, obtained dried shaping compound.
4th step, dried shaping compound is placed in resistance furnace, under 1330 ~ 1400 DEG C of conditions, is incubated 45 ~ 50 minutes, with stove naturally cooling, obtains mullite light refractory material.
Mullite light refractory material prepared by the present embodiment, after measured: yield rate is 98.0 ~ 98.2%; Volume density is 0.60 ~ 0.65gcm
-3; Cold crushing strength is 4.5 ~ 5.0MPa; Thermal conductivity is 0.18 ~ 0.19Wm
-1k
-1.
embodiment 4
A kind of mullite light refractory material and preparation method thereof.The concrete steps of described preparation method are:
The first step, under 40 ~ 50 DEG C of water bath condition, AC whipping agent, poly(oxyethylene glycol) 400, bicarbonate of ammonia and water are inserted in container, stir 15 ~ 20 minutes, obtained expanding foam solution.Wherein, AC whipping agent: poly(oxyethylene glycol) 400: bicarbonate of ammonia: the mass ratio of water is 1: (2 ~ 4): (2 ~ 4): (104 ~ 120).
Second step, by expanding foam solution, ρ-Al
2o
3stir 6 ~ 8 minutes with Coal gangue powder, add die for molding, the compound after obtained shaping.Wherein, expanding foam solution: ρ-Al
2o
3: the mass ratio of Coal gangue powder is (55 ~ 60): (2 ~ 3): 100.
3rd step, the compound after shaping is placed in vacuum freeze drier lyophilize 76 ~ 84 hours, obtained dried shaping compound.
4th step, dried shaping compound is placed in resistance furnace, under 1330 ~ 1400 DEG C of conditions, is incubated 45 ~ 50 minutes, with stove naturally cooling, obtains mullite light refractory material.
Mullite light refractory material prepared by the present embodiment, after measured: yield rate is 98.7 ~ 98.9%; Volume density is 0.65 ~ 0.80gcm
-3; Cold crushing strength is 5.0 ~ 6.5MPa; Thermal conductivity is 0.19 ~ 0.22Wm
-1k
-1.
embodiment 5
A kind of mullite light refractory material and preparation method thereof.The concrete steps of described preparation method are:
The first step, under 45 ~ 55 DEG C of water bath condition, AC whipping agent, poly(oxyethylene glycol) 400, bicarbonate of ammonia and water are inserted in container, stir 15 ~ 20 minutes, obtained expanding foam solution.Wherein, AC whipping agent: poly(oxyethylene glycol) 400: bicarbonate of ammonia: the mass ratio of water is 1: (3 ~ 5): (1 ~ 3): (80 ~ 96).
Second step, by expanding foam solution, ρ-Al
2o
3stir 5 ~ 7 minutes with Coal gangue powder, add die for molding, the compound after obtained shaping.Wherein, expanding foam solution: ρ-Al
2o
3: the mass ratio of Coal gangue powder is (50 ~ 55): (1 ~ 2): 100.
3rd step, the compound after shaping is placed in vacuum freeze drier lyophilize 72 ~ 80 hours, obtained dried shaping compound.
4th step, dried shaping compound is placed in resistance furnace, under 1280 ~ 1350 DEG C of conditions, is incubated 45 ~ 50 minutes, with stove naturally cooling, obtains mullite light refractory material.
Mullite light refractory material prepared by the present embodiment, after measured: yield rate is 98.3 ~ 98.5%; Volume density is 0.80 ~ 0.85gcm
-3; Cold crushing strength is 6.5 ~ 7.0MPa; Thermal conductivity is 0.22 ~ 0.23Wm
-1k
-1.
embodiment 6
A kind of mullite light refractory material and preparation method thereof.The concrete steps of described preparation method are:
The first step, under 45 ~ 55 DEG C of water bath condition, AC whipping agent, poly(oxyethylene glycol) 400, bicarbonate of ammonia and water are inserted in container, stir 15 ~ 20 minutes, obtained expanding foam solution.Wherein, AC whipping agent: poly(oxyethylene glycol) 400: bicarbonate of ammonia: the mass ratio of water is 1: (3 ~ 5): (1 ~ 3): (88 ~ 104).
Second step, by expanding foam solution, ρ-Al
2o
3stir 5 ~ 7 minutes with Coal gangue powder, add die for molding, the compound after obtained shaping.Wherein, expanding foam solution: ρ-Al
2o
3: the mass ratio of Coal gangue powder is (50 ~ 55): (2 ~ 3): 100.
3rd step, the compound after shaping is placed in vacuum freeze drier lyophilize 72 ~ 80 hours, obtained dried shaping compound.
4th step, dried shaping compound is placed in resistance furnace, under 1280 ~ 1350 DEG C of conditions, is incubated 45 ~ 50 minutes, with stove naturally cooling, obtains mullite light refractory material.
Mullite light refractory material prepared by the present embodiment, after measured: yield rate is 98.3 ~ 98.6%; Volume density is 0.85 ~ 0.90gcm
-3; Cold crushing strength is 7.0 ~ 7.5MPa; Thermal conductivity is 0.23 ~ 0.24Wm
-1k
-1.
embodiment 7
A kind of mullite light refractory material and preparation method thereof.The concrete steps of described preparation method are:
The first step, under 45 ~ 55 DEG C of water bath condition, AC whipping agent, poly(oxyethylene glycol) 400, bicarbonate of ammonia and water are inserted in container, stir 15 ~ 20 minutes, obtained expanding foam solution.Wherein, AC whipping agent: poly(oxyethylene glycol) 400: bicarbonate of ammonia: the mass ratio of water is 1: (3 ~ 5): (2 ~ 4): (96 ~ 112).
Second step, by expanding foam solution, ρ-Al
2o
3stir 5 ~ 7 minutes with Coal gangue powder, add die for molding, the compound after obtained shaping.Wherein, expanding foam solution: ρ-Al
2o
3: the mass ratio of Coal gangue powder is (55 ~ 60): (1 ~ 2): 100.
3rd step, the compound after shaping is placed in vacuum freeze drier lyophilize 76 ~ 84 hours, obtained dried shaping compound.
4th step, dried shaping compound is placed in resistance furnace, under 1330 ~ 1400 DEG C of conditions, is incubated 45 ~ 50 minutes, with stove naturally cooling, obtains mullite light refractory material.
Mullite light refractory material prepared by the present embodiment, after measured: yield rate is 98.8 ~ 99.0%; Volume density is 0.75 ~ 0.85gcm
-3; Cold crushing strength is 6.0 ~ 7.0MPa; Thermal conductivity is 0.21 ~ 0.23Wm
-1k
-1.
embodiment 8
A kind of mullite light refractory material and preparation method thereof.The concrete steps of described preparation method are:
The first step, under 45 ~ 55 DEG C of water bath condition, AC whipping agent, poly(oxyethylene glycol) 400, bicarbonate of ammonia and water are inserted in container, stir 15 ~ 20 minutes, obtained expanding foam solution.Wherein, AC whipping agent: poly(oxyethylene glycol) 400: bicarbonate of ammonia: the mass ratio of water is 1: (3 ~ 5): (2 ~ 4): (104 ~ 120).
Second step, by expanding foam solution, ρ-Al
2o
3stir 5 ~ 7 minutes with Coal gangue powder, add die for molding, the compound after obtained shaping.Wherein, expanding foam solution: ρ-Al
2o
3: the mass ratio of Coal gangue powder is (55 ~ 60): (2 ~ 3): 100.
3rd step, the compound after shaping is placed in vacuum freeze drier lyophilize 76 ~ 84 hours, obtained dried shaping compound.
4th step, dried shaping compound is placed in resistance furnace, under 1330 ~ 1400 DEG C of conditions, is incubated 45 ~ 50 minutes, with stove naturally cooling, obtains mullite light refractory material.
Mullite light refractory material prepared by the present embodiment, after measured: yield rate is 98.1 ~ 98.3%; Volume density is 0.90 ~ 0.95gcm
-3; Cold crushing strength is 7.5 ~ 8.0MPa; Thermal conductivity is 0.24 ~ 0.25Wm
-1k
-1.
This embodiment compared with prior art has the following advantages:
This embodiment adopts industrial solid castoff resource---and coal gangue is starting raw material, prepared mullite light refractory material with low cost.
This embodiment is without the need to special Preparation equipment and treatment technology, and save human resources, technical process is simple.
This embodiment, with " foaming " combination " vacuum lyophilization " technology, has ensured the froth stability of mullite light refractory material, has improve the yield rate of mullite light refractory material.
Mullite light refractory material prepared by this embodiment, after measured: yield rate is 98 ~ 99%; Volume density is 0.60 ~ 0.95gcm
-3; Cold crushing strength is 4.5 ~ 8.0MPa; Thermal conductivity is 0.18 ~ 0.25Wm
-1k
-1.
Therefore, this embodiment has with low cost, that technique is simple and yield rate is high feature; Prepared mullite light refractory material volume density is low, cold crushing strength is large and thermal conductivity is little.
Claims (8)
1. a preparation method for mullite light refractory material, is characterized in that the concrete steps of described preparation method are as follows:
The first step, under 40 ~ 55 DEG C of water bath condition, AC whipping agent, poly(oxyethylene glycol) 400, bicarbonate of ammonia and water are inserted in container, stir 15 ~ 20 minutes, obtained expanding foam solution; Wherein, AC whipping agent: poly(oxyethylene glycol) 400: bicarbonate of ammonia: the mass ratio of water is 1: (2 ~ 5): (1 ~ 4): (80 ~ 120);
Second step, by expanding foam solution, ρ-Al
2o
3stir 5 ~ 8 minutes with Coal gangue powder, add die for molding, the compound after obtained shaping; Wherein, expanding foam solution: ρ-Al
2o
3: the mass ratio of Coal gangue powder is (50 ~ 60): (1 ~ 3): 100;
3rd step, the compound after shaping is placed in vacuum freeze drier lyophilize 72 ~ 84 hours, obtained dried shaping compound;
4th step, dried shaping compound is placed in resistance furnace, under 1280 ~ 1400 DEG C of conditions, is incubated 45 ~ 50 minutes, with stove naturally cooling, obtains mullite light refractory material.
2. the preparation method of mullite light refractory material according to claim 1, is characterized in that described AC whipping agent is chemical pure, Cellmic C 121 content >=96wt%.
3. the preparation method of mullite light refractory material according to claim 1, is characterized in that described poly(oxyethylene glycol) 400 is analytical pure.
4. the preparation method of mullite light refractory material according to claim 1, is characterized in that described bicarbonate of ammonia is analytical pure.
5. the preparation method of mullite light refractory material according to claim 1, is characterized in that described ρ-Al
2o
3granularity≤0.1 μm of powder; Al
2o
3content>=99wt%.
6. the preparation method of mullite light refractory material according to claim 1, is characterized in that granularity≤40 μm of described Coal gangue powder; The main chemical compositions of coal gangue is: Al
2o
3content>=60wt%, SiO
2content>=25wt%, Fe
2o
3content≤2wt%, (K
2o+Na
2o) content≤0.5wt%.
7. the preparation method of mullite light refractory material according to claim 1, it is characterized in that the lyophilize temperature of described vacuum freeze drier is-40 ~-45 DEG C, vacuum pressure is 0.05 ~ 0.1Pa.
8. a mullite light refractory material, is characterized in that described mullite light refractory material is the mullite light refractory material prepared by preparation method of the mullite light refractory material according to any one of claim 1 ~ 7.
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