CN110256047A - A method of foamed ceramic is prepared using titanium-containing blast furnace slag and shale waste residue - Google Patents
A method of foamed ceramic is prepared using titanium-containing blast furnace slag and shale waste residue Download PDFInfo
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Abstract
The present invention relates to a kind of methods for preparing foamed ceramic using titanium-containing blast furnace slag and shale waste residue, sequentially include the following steps: S1, prepare titanium-containing blast furnace slag, shale waste residue, silicon dioxide powder as raw material;S2, prepare borax, ball clay, foaming agent, magnesia, manganese oxide and sodium metaphosphate as additive;S3, slurry is made in wet-milling after whole raw materials and additive mixing;S4, it slurry is put into baking oven is dried, then crushed in pulverizer, powder is made, diameter of particle is 200~300 mesh;S5, it powder granule is filled into after mold the temperature type resistance furnace in carries out roasting foaming and Crystallization Process;It is cooling later to obtain foamed ceramic.Method preparation process of the invention is succinct, easy to operate, and titanium-containing blast furnace slag and shale waste residue used is waste, realizes the resource utilization of solid waste, and obtained foamed ceramic value of the product is high.
Description
Technical field
The present invention relates to a kind of methods for preparing foamed ceramic using titanium-containing blast furnace slag and shale waste residue, belong to material preparation
Technical field.
Background technique
High temperature foamed ceramic has a large amount of closed pore, so having the performances such as lightweight, heat preservation, sound insulation, in addition ceramics are acidproof
Caustic corrosion, it is ageing-resistant, it is applied in many fields.The ratio applied in terms of building is wide: (1) can be prepared into
It is granular to be added in concrete, make building block loss of weight;(2) can be used to substitute traditional macromolecule wall heat insulation material, as outer
Materials for wall reaches insulation effect;(3) material that can be used as interior decoration, plays the role of heat preservation and soundproof.In some spies
Different field, such as military aspect, the filler that it can be used as hull play it is anti-settling, fire prevention, it is diamagnetic the effects of.Preparation foaming pottery
The method of porcelain is very more, and some of them is more complicated, but process flow is easier to control, so scholars are exploring
Foamed ceramic is prepared using cheap raw material, to widen its application.
There is vanadium titano-magnetite abundant in Panzhihua-Xichang Region, Panzhihua-Xichang Region v-ti magnetite ore reserves is close
10000000000 tons, association TiO28.7 hundred million tons, account for the 35.02% of World Titanium reserves.These resources are mainly deposited in the form of ilmenite
The titanium after ore dressing there are about 54% enters iron ore concentrate, and during blast furnace ironmaking, titanium substantially enters titanium-containing blast furnace slag.
Due to TiO in the titanium-containing blast furnace slag that discharges at present2Content be 23%~25%, and titaniferous ore disperse be distributed in clinker
In, it is difficult to separate, therefore the comprehensive utilization difficulty of titanium-containing blast furnace slag is larger.
Shale is a kind of sedimentary rock, complicated component, but all joints with thin laminated or thin slice stratiform, mainly by clay
The rock formed through pressure, temperature variation is deposited, in addition to clay mineral (such as kaolinite, hydromica, visits and carrys out stone at montmorillonite),
Also containing there are many detrital mineral (such as quartz, feldspar, mica) and authigenic mineral (such as oxides and hydroxide of iron, aluminium, manganese
Deng).Common kind is divided into black shale, culm, oil shale, siliceous shale, irony shale.Process of the shale in exploitation
In can generate waste residue, these waste residues hardly result in resource utilization, can only largely store up, and do not only take up large area soil, can also
Broken ring ecology, pollutes environment, how to efficiently use these waste residues is also that there is an urgent need for solve the problems, such as.
Summary of the invention
(1) technical problems to be solved
In order to solve the above problem of the prior art, the present invention provides a kind of to be prepared using titanium-containing blast furnace slag and shale waste residue
The method of foamed ceramic, using titanium-containing blast furnace slag, shale waste residue and silicon dioxide powder as raw material, borax, ball clay, foaming
Agent, magnesia, manganese oxide and sodium metaphosphate are as additive, through high-temperature roasting foaming, extensive resource utilization titaniferous
While blast furnace slag and shale waste residue, performance preferably foamed ceramic material is made.
(2) technical solution
In order to achieve the above object, the main technical schemes that the present invention uses include:
A method of foamed ceramic is prepared using titanium-containing blast furnace slag and shale waste residue comprising following steps:
S1, prepare titanium-containing blast furnace slag, shale waste residue, silicon dioxide powder as raw material;
S2, prepare borax, ball clay, foaming agent, magnesia, manganese oxide and sodium metaphosphate as additive;
S3, whole raw materials and additive are mixed to form mixed material, then carry out wet-milling with ball mill, be uniformly mixed simultaneously
Slurry is made;
S4, it slurry is put into baking oven being dried, then crushed in pulverizer, be made powder, diameter of particle is 200~
300 mesh;
S5, by powder filled into mold, be subsequently placed in middle temperature type resistance furnace, carry out roasting foaming and crystallization mistake
Journey;It is cooling later to obtain foamed ceramic.
In a preferred embodiment, in step sl, the titanium-containing blast furnace slag contains SiO by mass percentage2
28~29%, Al2O314~15%, Fe2O31~2%, CaO 26~27%, Na2O 0.03~0.04%, TiO219~
20%, MgO 7~8%, K2O 0.7~0.8%, remaining is impurity.
In a preferred embodiment, in step sl, the shale waste residue contains SiO by mass percentage2 66
~67%, Al2O315~16%, Fe2O35~6%, CaO 5~6%, Na2O 0.1~0.2%, TiO20.8~0.9%,
MgO 3~4%, K2O 1~2%, remaining is impurity.
In a preferred embodiment, in step sl, titanium-containing blast furnace slag 10 by mass percentage in the raw material
~27%, shale waste residue accounts for 60~79%, and silicon dioxide powder accounts for 12~17%.
In a preferred embodiment, in step s 2, the borax accounts for the 2~4% of total mass of raw material, ball clay
Account for the 3~5% of total mass of raw material, foaming agent accounts for the 0.3~0.5% of total mass of raw material, magnesia account for total mass of raw material 0.3~
0.7%, manganese oxide accounts for the 0.5~1% of total mass of raw material, and sodium metaphosphate accounts for the 0.5~1% of total mass of raw material.
In a preferred embodiment, in step s3, when the wet-milling mixed material, mill ball and water quality
Than for material: ball: water=1:1.8~2.4:0.6~1.0.
In a preferred embodiment, in step s 4, the drying dry 12~16h at 100~120 DEG C.
In a preferred embodiment, in step s 5, the temperature schedule in the roasting foaming and Crystallization Process
Are as follows: furnace temperature is raised to 850~950 DEG C from room temperature with the rate of 8~10 DEG C/min, at least 30min is kept the temperature, then with 2~4 DEG C/min
Heating rate be raised to 1050~1100 DEG C, keep the temperature 30~60min.
Through lot of experiment validation, TiO in titanium-containing blast furnace slag used in the present invention2Content is higher, TiO2It can be used as induction analysis
Brilliant nucleus, to reach the condition for preparing foamed ceramic;SiO in shale waste residue2Content is higher, the more fusing point of quartz mineral compared with
Height, and CaO, Al in titanium-containing blast furnace slag2O3Content is higher, according to SiO2-CaO-Al2O3Ternary phase diagrams obtains: when three constituent elements reach
SiO when to eutectic point2Content is 63% or so.Calculation shows that titanium-containing blast furnace slag, shale waste residue and silicon dioxide powder are pressed
(10~27%): (60~79%): (12~17%) ratio is mutually adulterated, and additional suitable fluxing agent (borax) can make original
Expect congruent melting at a lower temperature, if the ratio of three is higher or lower than above-mentioned condition, the eutectic temperature of raw material can be made significantly
It improves;Only with can be obtained by primary roasting, bulk density is small, and intensity is high, heat-insulated for the mixture that method of the invention obtains
The good high-performance foamed ceramic of performance.
The bulk density for the foamed ceramic that the method for the present invention prepares is 0.216~0.398g/cm3, compression strength is
2.231~4.266MPa, thermal coefficient are 0.04~0.09W/ (mK).
(3) beneficial effect
The beneficial effects of the present invention are:
Method of the invention prepares the range of choice that foamed ceramic expands raw material using shale waste residue as primary raw material, drop
Low production cost has huge facilitation to the energy conservation of building.
The method have the advantages that:
1) experimental implementation is simple, not complicated step;
2) titanium-containing blast furnace slag and shale waste residue are solid waste, realize the resource utilization of solid waste, obtain
Foamed ceramic value of the product it is high;
3) it is only fired with a step, the foaming and controlled micro crystallization of foamed ceramic can be completed, cost substantially reduces, by testing
Card, foamed ceramic are had excellent performance, and reach the standard (thermal coefficient≤0.05W/ (mK)) of national efficient thermal insulation material.
The method provided by the invention for preparing foamed ceramic using titanium-containing blast furnace slag and shale waste residue is easy to implement industrialization,
The use of solid waste is raw material, meets the demand for development of national energy conservation and emission reduction, can realize that large area is once burnt in tunnel oven
At any cutting as requested can be in heat preserving and insulating material, and fire proofing material, the fields such as construction material are used widely.
Specific embodiment
In order to preferably explain the present invention, in order to understand, below by specific embodiment, present invention work is retouched in detail
It states.Wherein, partial size≤0.074mm of mixture used in the examples;The titanium-containing blast furnace slag of use contains by mass percentage
SiO228~29%, Al2O314~15%, Fe2O31~2%, CaO 26~27%, Na2O 0.03~0.04%, TiO2 19
~20%, MgO 7~8%, K2O 0.7~0.8%, remaining is impurity.The shale waste residue of use contains by mass percentage
SiO266~67%, Al2O315~16%, Fe2O35~6%, CaO 5~6%, Na2O 0.1~0.2%, TiO20.8~
0.9%, MgO 3~4%, K2O 1~2%, remaining is impurity.
Magnesia, manganese oxide, silicon dioxide powder and the sodium metaphosphate used in the following examples of the present invention is commercially available production
Product.The mass ratio of mixture, mill ball and water is material: ball: water=1:(1.8~2.4 when ball milling): (0.6~1.0);Mold is
Pin-connected panel refractory brick kiln furnitures;The heating furnace used is middle temperature type resistance furnace.
Embodiment 1
The method for preparing foamed ceramic using titanium-containing blast furnace slag and shale waste residue, using following steps:
(1) prepare titanium-containing blast furnace slag, shale waste residue, silicon dioxide powder as raw material, by mass percentage: titaniferous
Blast furnace slag accounts for 26.09%, and shale waste residue accounts for 60.87%, and silicon dioxide powder accounts for 13.04%;These raw materials are mixed, by mixture
Partial size it is levigate to partial size≤0.074mm;
(2) prepare borax, ball clay, foaming agent, magnesia, manganese oxide and sodium metaphosphate as additive;In additive
Borax accounts for 4% of total mass of raw material in step (1), and ball clay accounts for 4% of total mass of raw material in step (1), and foaming agent accounts for step
(1) the 0.3% of total mass of raw material in, magnesia account for 0.5% of total mass of raw material in step (1), and manganese oxide accounts for step (1) Central Plains
Expect the 1% of gross mass, sodium metaphosphate accounts for 1% of total mass of raw material in step (1);
(3) by step (1) raw material and additive be mixed to form mixed material, then carry out wet-milling with ball mill, mix
It closes uniformly and slurry is made;The mass ratio of mixture, mill ball and water is material: ball: water=1:2:0.6 when ball milling;
(4) slurry is put into baking oven to be dried, the dry 12h at 120 DEG C is dried for the uniformity for guaranteeing slurry
Cheng Zhongxu is stirred, and is then crushed in pulverizer, and powder is made, and diameter of particle is 200~300 mesh;
(5) it by powder filled into mold, is subsequently placed in middle temperature type resistance furnace, carries out roasting foaming pore-creating;Roasting
Temperature schedule in foaming poration process are as follows: furnace temperature is raised to 900 DEG C from room temperature with the rate of 8 DEG C/min, keeps the temperature 30min, then
1070 DEG C are raised to the heating rate of 3 DEG C/min, keeps the temperature 60min;
(6) room temperature is cooled to the furnace after the completion of roasting foaming pore-creating, obtain foamed ceramic material;It is drained using Archimedes
The bulk density of method measurement sample.Thermal coefficient uses " GB/T 10294-2008 Technology of Steady State Thermal Resistance of Thermal Insulating Material and related characteristic
Measurement Guarded hot plate " be measured.Using full-automatic pressure testing machine, (industrial test system is created in Jinan to be had compression strength
Limit company, ZCQT-S50kN type) measurement, compression face size is about 80mm × 80mm, thickness of sample 80mm.It will test, foam
The bulk density of ceramic material is 0.371g/cm3, compression strength 4.023MPa, thermal coefficient is 0.08W/ (mK).
Embodiment 2
With embodiment 1, difference is method:
(1) titanium-containing blast furnace slag accounts for 17.39% by mass percentage in raw material, and shale waste residue accounts for 69.57%, silicon dioxide powder
Account for 13.04%;
(2) 900 DEG C are raised to the rate of 9 DEG C/min, keep the temperature 30min, be raised to 1070 DEG C with the rate of 3 DEG C/min, heat preservation
60min。
The foamed ceramic material of acquisition, its bulk density is 0.216g/cm after measured3, compression strength 2.231MPa leads
Hot coefficient is 0.04W/ (mK).
Embodiment 3
With embodiment 1, difference is method:
(1) titanium-containing blast furnace slag accounts for 8.70% by mass percentage in raw material, and shale waste residue accounts for 78.26%, silicon dioxide powder
Account for 13.04%;
(2) 900 DEG C are raised to the rate of 9 DEG C/min, keep the temperature 30min, be raised to 1060 DEG C with the rate of 3 DEG C/min, heat preservation
60min。
Foamed ceramic material is obtained, its bulk density is 0.398g/cm after measured3, compression strength 4.266MPa is thermally conductive
Coefficient is 0.09W/ (mK).
Embodiment 4
The method for preparing foamed ceramic using titanium-containing blast furnace slag and shale waste residue, using following steps:
(1) prepare titanium-containing blast furnace slag, shale waste residue, silicon dioxide powder as raw material, titaniferous by mass percentage in raw material
Blast furnace slag accounts for 17.39%, and shale waste residue accounts for 69.57%, and silicon dioxide powder accounts for 13.04%;Borax accounts for the total matter of raw material in additive
The 3.5% of amount, ball clay accounts for the 5% of total mass of raw material, and foaming agent accounts for the 0.4% of total mass of raw material, and magnesia accounts for the total matter of raw material
The 0.7% of amount, manganese oxide accounts for the 0.8% of total mass of raw material, and sodium metaphosphate accounts for the 0.8% of total mass of raw material;
(2) whole raw materials and additive are mixed to form mixed material, then carry out wet-milling with ball mill, mixture is ground
The mass ratio of abrading-ball and water is material: ball: water=1:2:0.6, and Ball-milling Time 5min is uniformly mixed and slurry is made;
(3) by step (1) raw material and additive be mixed to form mixed material, then carry out wet-milling with ball mill, mix
It closes uniformly and slurry is made;The mass ratio of mixture, mill ball and water is material: ball: water=1:2:0.6 when ball milling;
(4) slurry is put into baking oven to be dried, the dry 12h at 120 DEG C is dried for the uniformity for guaranteeing slurry
Cheng Zhongxu is stirred, and is then crushed in pulverizer, and powder is made, and diameter of particle is 200~300 mesh;
(5) powder is roasted, is raised to 950 DEG C with the rate of 9 DEG C/min, 30min is kept the temperature, then with 3 DEG C/min's
Heating rate is raised to 1070 DEG C, keeps the temperature 30min.
Foamed ceramic material obtained, its bulk density is 0.349g/cm after measured3, compression strength 3.798MPa leads
Hot coefficient is 0.08W/ (mK).
Embodiment 5
The method for preparing foamed ceramic using titanium-containing blast furnace slag and shale waste residue, using following steps:
(1) using titanium-containing blast furnace slag, shale waste residue, silicon dioxide powder as raw material, titaniferous is high by mass percentage in raw material
Clinker accounts for 17.39%, and shale waste residue accounts for 69.57%, and silicon dioxide powder accounts for 13.04%;Borax accounts for total mass of raw material in additive
3%, ball clay accounts for the 5% of total mass of raw material, and foaming agent accounts for the 0.3% of total mass of raw material, and magnesia accounts for total mass of raw material
0.6%, manganese oxide accounts for the 0.5% of total mass of raw material, and sodium metaphosphate accounts for the 0.5% of total mass of raw material;
(2) by step (1) raw material and additive be mixed to form mixed material, then carry out wet-milling with ball mill, mix
It closes uniformly and slurry is made;The mass ratio of mixture, mill ball and water is material: ball: water=1:2:0.6 when ball milling;
(3) slurry is put into baking oven to be dried, the dry 12h at 120 DEG C is dried for the uniformity for guaranteeing slurry
Cheng Zhongxu is stirred, and is then crushed in pulverizer, and powder is made, and diameter of particle is 200~300 mesh;
(4) it by powder filled into mold, is subsequently placed in middle temperature type resistance furnace, carries out roasting foaming pore-creating;Roasting
Temperature schedule in foaming poration process are as follows: furnace temperature is raised to 950 DEG C from the rate of 9 DEG C/min, 30min is kept the temperature, then with 2
DEG C/heating rate of min is raised to 1070 DEG C, keep the temperature 50min.
Foamed ceramic material obtained, its bulk density is 0.235g/cm after measured3, compression strength 2.969MPa leads
Hot coefficient is 0.05W/ (mK).
Comparative example
It uses and prepares foamed ceramic using high silicon tailings, steel-making tailings, shale and kaolin as raw material in the prior art, use
Detection method in above-described embodiment 1, the bulk density of obtained foamed ceramic are 0.2~0.4g/cm3, compression strength 1.5
~2.0MPa, thermal coefficient are 0.06~1W/ (mK).
Can be seen that from above-described embodiment foamed ceramic bulk density that method of the invention obtains be 0.216~
0.398g/cm3, compression strength is 2.231~4.266MPa, and thermal coefficient is 0.04~0.09W/ (mK), and comprehensive performance is wanted
Higher than the prior art.
The above described is only a preferred embodiment of the present invention, being not the limitation for doing other forms to the present invention, appoint
What those skilled in the art can use the equivalence enforcement that technology contents disclosed above were changed or be modified as equivalent variations
Example.But without departing from the technical solutions of the present invention, according to the technical essence of the invention to the above embodiments
What simple modification, equivalent variations and remodeling, still falls within the protection scope of technical solution of the present invention.
Claims (8)
1. a kind of method for preparing foamed ceramic using titanium-containing blast furnace slag and shale waste residue, which is characterized in that it includes following step
It is rapid:
S1, prepare titanium-containing blast furnace slag, shale waste residue, silicon dioxide powder as raw material;
S2, prepare borax, ball clay, foaming agent, magnesia, manganese oxide and sodium metaphosphate as additive;
S3, whole raw materials and additive are mixed to form mixed material, then carry out wet-milling with ball mill, be uniformly mixed and be made
Slurry;
S4, it slurry is put into baking oven is dried, then crushed in pulverizer, powder is made, diameter of particle is 200~300
Mesh;
S5, by powder filled into mold, be subsequently placed in middle temperature type resistance furnace, carry out roasting foaming and Crystallization Process;It
It is cooling afterwards to obtain foamed ceramic.
2. the method as described in claim 1, which is characterized in that in step sl, the titanium-containing blast furnace slag is by mass percentage
Meter contains SiO228~29%, Al2O314~15%, Fe2O31~2%, CaO 26~27%, Na2O 0.03~0.04%,
TiO219~20%, MgO 7~8%, K2O 0.7~0.8%, remaining is impurity.
3. the method as described in claim 1, which is characterized in that in step sl, the shale waste residue is by mass percentage
Containing SiO266~67%, Al2O315~16%, Fe2O35~6%, CaO 5~6%, Na2O 0.1~0.2%, TiO2 0.8
~0.9%, MgO 3~4%, K2O 1~2%, remaining is impurity.
4. the method as described in claim 1, which is characterized in that in step sl, titaniferous by mass percentage in the raw material
Blast furnace slag 10~27%, shale waste residue account for 60~79%, and silicon dioxide powder accounts for 12~17%.
5. the method as described in claim 1, which is characterized in that in step s 2, the borax account for total mass of raw material 2~
4%, ball clay accounts for the 3~5% of total mass of raw material, and foaming agent accounts for the 0.3~0.5% of total mass of raw material, and it is total that magnesia accounts for raw material
The 0.3~0.7% of quality, manganese oxide account for the 0.5~1% of total mass of raw material, and sodium metaphosphate accounts for the 0.5~1% of total mass of raw material.
6. the method as described in claim 1, which is characterized in that in step s3, the mixed material when wet-milling, mill ball and
The mass ratio of water is material: ball: water=1:1.8~2.4:0.6~1.0.
7. the method as described in claim 1, which is characterized in that in step s 4, the drying is dry at 100~120 DEG C
12~16h.
8. method as described in any of claims 17, which is characterized in that in step s 5, the roasting foaming and crystallization
Temperature schedule in the process are as follows: furnace temperature is raised to 850~950 DEG C from room temperature with the rate of 8~10 DEG C/min, keeps the temperature at least 30min,
Then 1050~1100 DEG C are raised to the heating rate of 2~4 DEG C/min, keep the temperature 30~60min.
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CN112898045A (en) * | 2021-03-31 | 2021-06-04 | 成渝钒钛科技有限公司 | High-titanium blast furnace slag porous sound-absorbing ceramic and preparation method thereof |
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CN116606161A (en) * | 2023-05-25 | 2023-08-18 | 攀枝花学院 | Method for preparing porous ceramic from titanium-containing blast furnace slag and silicon slag |
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