CN106146027A - Foamed ceramics walling with slag as raw material and preparation method thereof - Google Patents
Foamed ceramics walling with slag as raw material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/131—Inorganic additives
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1321—Waste slurries, e.g. harbour sludge, industrial muds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1321—Waste slurries, e.g. harbour sludge, industrial muds
- C04B33/1322—Red mud
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/135—Combustion residues, e.g. fly ash, incineration waste
- C04B33/1352—Fuel ashes, e.g. fly ash
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/138—Waste materials; Refuse; Residues from metallurgical processes, e.g. slag, furnace dust, galvanic waste
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/02—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding chemical blowing agents
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3436—Alkaline earth metal silicates, e.g. barium silicate
- C04B2235/3445—Magnesium silicates, e.g. forsterite
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- C—CHEMISTRY; METALLURGY
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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- Engineering & Computer Science (AREA)
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- Environmental & Geological Engineering (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
- Processing Of Solid Wastes (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention provides a kind of foamed ceramics walling with slag as raw material, it is mainly by made by the raw material of following weight ratio: 22~66 parts of slags, 24~50 parts of rich aluminium wastes, 10~28 parts of rich magnesium materials, additional 6~18 biological materials, 3~10 parts of foaming agent;By mixing, ball milling, molding, burn till prepared at 1020 DEG C~1250 DEG C, it is achieved that prepare foamed ceramics walling at low temperatures.The foamed ceramics walling production cost that the present invention makes is low, turn waste into wealth, and discontinuous between pore, does not absorbs water, and porosity of holding one's breath is high, water absorption rate is low, the more high characteristic of comprcssive strength, is the insulation walling of a kind of function admirable.
Description
Technical field
The invention belongs to inorganic heat insulation material field.Be specifically related to a kind of foamed ceramics walling with slag as raw material and
Preparation method.
Background technology
The iron and steel output of China is constantly in the first in the world over nearly 10 years, and within 2009, China's output of steel has reached 5.65 hundred million t.Often
Refining 100t steel will produce 10t to 15t slag, and China's steel slag utilization approach has: melts down sintering and utilizes, builds the road, engineering backfill material,
Preparation cement, does other building materials etc..But by resource and effectiveness evaluation, it is left that China's slag practical efficiency is only 10%
The right side, the slag not utilized takies a large amount of soil and serious environment pollution.If slag can be made to become a kind of new mineral admixture,
Not only significant to sustainable development, it is possible to be substantially reduced building materials industry cost.To its comprehensive utilization, it is allowed to turn waste into wealth
It it is the requirement of sustainable development.Patent " a kind of method utilizing metallurgical steel slag to produce Ceramic Tiles " (CN101386528), " a kind of
The floor tile (CN104944917A) etc. that doping slag intensity is high;These methods all can recycle slag, but product is attached
Value added low.Therefore, it is necessary to exploitation utilizes slag and the high new product of added value of product in a large number.
Along with the fast development of China's economy, the progressively improvement of people's life, with from the quick demand of building, building
Sustainable growth, energy resource consumption will be greatly improved by energy consumption, and building energy conservation and Development of Novel materials for wall become implements economic development
One major issue of strategy, is social progress and the important ring increased economic efficiency, and wherein closed cell foamed ceramics is as Novel wall
Body material not only has the critical functions such as insulation, fire prevention, heat insulation, sound insulation, corrosion-resistant, humidity, also has that water absorption rate is low, resistance to compression
High, rate of closed hole high, has boundless prospect at building field.Patent CN104529510A mixes foaming with coal dust
As fuel in ceramic batch, it is prepared for foamed ceramic, reduces energy consumption and cost.Patent CN104557120A is with about 60%
Gangue is main material, adds the foaming agent such as sandstone, Anhydrite, dolomite, graphite and calcium carbonate, prepares external wall foamed ceramic
Insulation material.
The excellent thermal and insulating performance of closed cell foamed ceramics is for the significance of building energy conservation, to closed cell foamed ceramics
Research and development of products is more and more paid attention to, and the most only foam process is the more ripe one preparing closed cell foamed ceramics at present
Method.Compared with other preparation technologies, it is relatively easy to control the shape of ceramic, porosity and unit weight, and applicable production is held one's breath
The ceramic material in hole.
Summary of the invention
Goal of the invention: for the problem of existence of the prior art, the present invention is on original basis preparing foamed ceramics
On, consider that selecting slag, rich aluminium waste, rich magnesium material is primary raw material from production cost, it is provided that a kind of rate of closed hole high structure
The closed cell foamed ceramics being evenly distributed.
It is equal that another object of the present invention is to provide one to prepare described rate of closed hole high structure distribution at a lower temperature
The method of even closed cell foamed ceramics, and simple to operate, it is easy to technology controlling and process.
Technical scheme: the invention provides a kind of foamed ceramics walling with slag as raw material, between described walling pore
Discontinuous, do not absorb water, and the characteristics such as porosity is high, water absorption rate is low, comprcssive strength is higher, density is little of holding one's breath, it is that a kind of performance is excellent
Good heat preserving and insulating material, it is mainly by made by the raw material of following weight ratio: 22~66 parts of slags, 24~50 parts of rich aluminum
Waste material, 10~28 parts of rich magnesium materials, additional 6~18 biological materials, 3~10 parts of foaming agent;Each component content in described slag:
SiO2Be 13.56~14.78%, MgO be 1.59~8.1%, Fe2O3Be 8.12~9.21%, Al2O3Be 3.17~5.16%,
CaO be 40~58.21% and K, Na less than 3%.
Described rich aluminium waste is the one in gangue, red mud, mud, fluid bed coal ash.Wherein gangue, red mud, dirt
Clay sculpture is preferable.
Described rich magnesium material is the one in Talcum, silicon manganese slag, magnesium slag
Described biomass material is the one in straw, rice husk.
Described foaming agent is one or more mixing in iron sesquioxide, sodium carbonate, carbon dust.
The water absorption rate of described foamed ceramics walling is less than 3%, and density is less than 200kg/m3, comprcssive strength be 7.53MPa~
16.00MPa, porosity of holding one's breath is 49~90%.
Present invention also offers the preparation method of above-mentioned foamed ceramics walling, it is characterised in that mainly comprise the steps that
(1) slag crushing grinding 0.5~4h, obtain slag powder body;
(2) slag 22~66 parts, rich aluminium waste 24~50 parts, rich magnesium material 10~28 parts, additional biology are weighed by formula
Material 6~18 parts, foaming agent 3~10 parts of mixing, ball millings obtain mixed powder, pack standby.Ball milling can make foaming agent equal
Even being distributed in powder, this is the necessary requirement obtaining the uniform foamed ceramic of bubble diameter.
(3) powder body that step (2) prepares is added water or industrial wastes, mixing, molding, obtain base substrate.When plasticity is inadequate
Being preferably added to industrial wastes, described industrial wastes, in spent pulping liquor, sugar waste, waste leather-making liquid, wine brewing waste liquid
Kind.Described forming method uses extrusion molding or compression molding.
(4) green compact are placed in saggar, are placed in high temperature furnace, process with certain heating schedule, to obtain final product.
Heating schedule in described step (4) is:: with the speed of 2~6 DEG C/min by room temperature to 500 DEG C, it is incubated 50
~60min, then rise to 1020 DEG C~1250 DEG C with the programming rate of 3~7 DEG C/min, it is incubated 120~180min.
One preferred plan of the present invention is: 66 parts of slags, 24 parts of rich aluminium wastes, 10 parts of rich magnesium materials, additional 6 parts of biologies
Material, 10 parts of foaming agent, calcining system: 20 DEG C~500 DEG C, intensification 96min, 500 DEG C of insulation 1h, 500 DEG C~1250 DEG C, rise
Temperature 120min, 1250 DEG C of insulation 2h, naturally cool to room temperature.
In described preferred plan, preferred formula is: 66 parts of slags, 24 parts of gangues, 10 parts of Talcums, additional 6 parts of straws, 7
Part iron sesquioxide and 3 parts of carbon dusts, wherein straw adds iron sesquioxide and carbon dust foaming effect is optimal, can form pore-size distribution equal
Even, that rate of closed hole is high foamed ceramics walling.
Beneficial effect: the foamed ceramics walling that (1) present invention develops is prepared at low temperatures and reduced production cost, shape simultaneously
Between the pore become discontinuous based on closed pore, the excellent properties such as water absorption rate is low, density is little, comprcssive strength is big, can extensively answer
For insulation walling.
(2) the raw materials used predominantly industrial solid castoff of the present invention, low production cost, can reduce environment simultaneously
Pollute, improve the comprehensive utilization to waste residue.
(3) biological material used by the present invention not only can reduce firing temperature and also can as a kind of pore creating material,
Improve the comprehensive utilization to crops simultaneously.
(4) foaming agent of the present invention simply and easily obtains. during easy fired, foaming agent is decomposed
Or reduction reaction generates gas, causing material to foam, foaming process is slow, and does not have persistence, along with the liter of firing temperature
Height, glass increases mutually, promotes sintering, causes pore volume to tend to reducing, and porosity of holding one's breath raises, and pore independence is good, aperture
It is evenly distributed.
Detailed description of the invention:
Referring to specific embodiment, the present invention is described.Only it will be appreciated by those skilled in the art that these embodiments
For the present invention is described, it limits the scope of the present invention never in any form.
Raw material used in following embodiment, reagent material etc., if no special instructions, be commercially available purchase product.
Embodiment 1
Designed by the present embodiment, proportioning raw materials is as shown in table 1.
Table 1 embodiment 1 proportioning raw materials
Embodiment 1 | Slag: gangue: Talcum | Additional straw: iron sesquioxide: carbon dust |
Mass ratio | 66:24:10 | 6:7:3 |
It is embodied as step as follows:
Ball mill mixing: slag, gangue, Talcum 66:24:10 in mass ratio is weighed, additional 6 parts of straws, 7 part of three oxidation
Two and 3 parts of carbon dusts, ball milling 2h, add water mixing;
Molding: extrusion molding, obtains base substrate;
Burn till: 20 DEG C~500 DEG C, intensification 96min, 500 DEG C of insulation 1h, 500 DEG C~1250 DEG C, intensification 120min, 1250
DEG C insulation 2h, naturally cool to room temperature.
Performance test: use Archimedes' principle record the porosity of holding one's breath of foamed ceramics be 90%, water absorption rate 1.1%, close
Degree 160kg/m3, using universal testing machine to record its comprcssive strength is 16.00Mpa.
Embodiment 2
Designed by the present embodiment, proportioning raw materials is as shown in table 2.
Table 2 embodiment 2 proportioning raw materials
Embodiment 2 | Slag: fluid bed coal ash: silicon manganese slag | Additional straw: iron sesquioxide |
Mass ratio | 22:50:28 | 18:3 |
It is embodied as step as follows:
Ball mill mixing: slag, fluid bed coal ash, silicon manganese slag 22:50:28 in mass ratio are weighed, additional 18 parts of straws, 3
Part iron sesquioxide, ball milling 2h;
Molding: additional spent pulping liquor makees binding agent, extrusion molding, obtains base substrate;
Burn till: 20 DEG C~500 DEG C, intensification 96min, 500 DEG C of insulation 1h, 500 DEG C~1020 DEG C, intensification 120min, 1020
DEG C insulation 120min, naturally cool to room temperature.
Performance test: use Archimedes' principle record the porosity of holding one's breath of foamed ceramics be 86%, water absorption rate 2.1%, close
Degree 180kg/m3, using universal testing machine to record its comprcssive strength is 10.32Mpa.
Embodiment 3
Designed by the present embodiment, proportioning raw materials is as shown in table 3.
Table 3 embodiment 3 proportioning raw materials
It is embodied as step as follows:
Ball mill mixing: slag, calcium enriched cyclone-furnace slag, magnesium slag 44:37:19 in mass ratio are weighed, additional 12 parts of straws, 4 parts
Iron sesquioxide and 2.5 parts of carbon dusts, ball milling 2h;
Molding: additional sugar waste makees binding agent, compression molding under 5MPa, obtain base substrate;
Burn till: 20 DEG C~500 DEG C, intensification 96min, 500 DEG C of insulation 1h, 500 DEG C~1165 DEG C, intensification 100min, 1165
DEG C insulation 120min, naturally cool to room temperature.
Performance test: use Archimedes' principle record the porosity of holding one's breath of foamed ceramics be 49%, water absorption rate 2.48%, close
Degree 200kg/m3, using universal testing machine to record its comprcssive strength is 7.53Mpa.
Embodiment 4
Designed by the present embodiment, proportioning raw materials is as shown in table 4.
Table 4 embodiment 4 proportioning raw materials
Embodiment 4 | Slag: red mud: magnesium slag | Additional straw: sodium carbonate |
Mass ratio | 30:50:20 | 2:3 |
It is embodied as step as follows:
Ball mill mixing: slag, red mud, magnesium slag 30:50:20 in mass ratio are weighed, additional 2 parts of straws, 3 parts of sodium carbonate,
Ball milling 2h, add water mixing;
Molding: extrusion molding, obtains base substrate;
Burn till: 20 DEG C~500 DEG C, intensification 96min, 500 DEG C of insulation 50min, 500 DEG C~1100 DEG C, intensification 100min,
1100 DEG C of insulation 150min, naturally cool to room temperature.
Performance test: use Archimedes' principle record have the porosity of holding one's breath of foamed ceramics be 78.54%, water absorption rate
2.57%, density 178kg/m3, using universal testing machine to record its comprcssive strength is 11.25MPa.
Embodiment 5
Designed by the present embodiment, proportioning raw materials is as shown in table 5.
Table 5 embodiment 5 proportioning raw materials
Embodiment 5 | Slag: mud: Talcum | Additional rice husk: carbon dust |
Mass ratio | 60:25:15 | 5:1 |
It is embodied as step as follows:
Ball mill mixing: slag, mud, Talcum 60:25:15 in mass ratio is weighed, additional 5 parts of rice husks, 1 part of carbon dust, ball
Mill 2h, add water mixing;
Molding: compression molding under 6MPa, obtains base substrate;
Burn till: 20 DEG C~500 DEG C, intensification 96min, 500 DEG C of insulation 1h, 500 DEG C~1200 DEG C, intensification 120min, 1200
DEG C insulation 150min, naturally cool to room temperature.
Performance test: use Archimedes' principle record have the porosity of holding one's breath of foamed ceramics be 72.26%, water absorption rate
3%, 148kg/m3, using universal testing machine to record its comprcssive strength is 9.43Mpa.
Claims (9)
1. the foamed ceramics walling with slag as raw material, it is characterised in that described walling, it is mainly by following weight part ratio
Made by the raw material of example: 22~66 parts of slags, 24~50 parts of rich aluminium wastes, 10~28 parts of rich magnesium materials, additional 6~18 biomass
Material, 3~10 parts of foaming agent;Each component content: SiO in described slag2Be 13.56~14.78%, MgO be 1.59~
8.1%, Fe2O3Be 8.12~9.21%, Al2O3Be 3.17~5.16%, CaO be 40~58.21% and K, Na less than 3%.
2. such as the foamed ceramics walling in claim 1, it is characterised in that described rich aluminium waste is gangue, red mud, mud, stream
Change the one in bed coal ash.
3. such as the foamed ceramics walling in claim 1, it is characterised in that described rich magnesium material is in Talcum, silicon manganese slag, magnesium slag
One.
4. such as the foamed ceramics walling in claim 1, it is characterised in that described biomass material is in straw, rice husk
Kind.
5. such as the foamed ceramics walling in claim 1, it is characterised in that described foaming agent is iron sesquioxide, carbon dust, carbonic acid
One or more mixing in sodium.
6. the preparation method of foamed ceramics walling described in claim 1, it is characterised in that mainly comprise the steps that
(1) slag crushing grinding 0.5~4h, obtain slag powder body;
(2) slag 22~66 parts, rich aluminium waste 24~50 parts, rich magnesium material 10~28 parts, additional biomass material are weighed by formula
Expect that 6~18 parts, foaming agent 3~10 parts of mixing, ball millings obtain mixed powder, pack standby;
(3) powder body that step (2) prepares is added water or industrial wastes, mixing, molding, obtain base substrate;
(4) green compact are placed in saggar, are placed in high temperature furnace, process with certain heating schedule in atmosphere, to obtain final product.
Preparation method the most according to claim 6, it is characterised in that the industrial wastes described in described step (3) is paper pulp
One in waste liquid, sugar waste, waste leather-making liquid, wine brewing waste liquid.
Preparation method the most according to claim 6, it is characterised in that in described step (3), forming method uses extrusion molding
Or compression molding.
Preparation method the most according to claim 6, it is characterised in that the heating schedule in described step (4) is: with 2~6
DEG C/speed of min by room temperature to 500 DEG C, be incubated 50~60min, then rise to 1020 with the programming rate of 3~7 DEG C/min
DEG C~1250 DEG C, be incubated 120~180min.
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