CN109553424B - Fiber-reinforced high-temperature-resistant light high-alumina foaming coating material - Google Patents
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/10—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by using foaming agents or by using mechanical means, e.g. adding preformed foam
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- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- 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
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
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- 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
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5212—Organic
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Abstract
A high-temp-resistant light high-alumina foaming coating material with fibre reinforcement is prepared from high-alumina bauxite powder, silicon powder and alumina powder. The aluminum sol and the calcium aluminate cement are used as a bonding agent, and the zirconium aluminate refractory fiber is added, so that the use temperature can reach 1420 ℃. The invention has simple preparation process, saves the step of preparing foam in advance, and is convenient to use immediately after preparation on site during construction. The invention can produce strength after being rapidly cured within 30-65min, and can reasonably control the construction time. The invention can adapt to the construction of special-shaped areas of the kiln, such as corners, grooves and round outer walls, and avoids the phenomenon that the heat insulation material at the special-shaped part of the kiln is not tightly contacted with the kiln and falls off and loosens.
Description
Technical Field
The invention belongs to the technical field of production of heat-insulating and heat-preserving refractory materials, and particularly relates to a fiber-reinforced high-temperature-resistant light high-alumina foaming coating material.
Background
The heat preservation of the kiln can effectively reduce the heat loss in the kiln, and the consumption of fuel is saved. At present, the calcium silicate board has better heat preservation effect in the high-temperature kiln, because the volume density of the calcium silicate board is far less than that of a light refractory heat-insulating refractory material, and the heat conductivity coefficient is also far less than that of the heat-insulating refractory material. However, calcium silicate boards currently face the following problems: (1) under the condition of high temperature, the service performance is reduced, the aging of the material is accelerated, and the heat conductivity coefficient is increased. At present, the use temperature of the calcium silicate board is in the range of 800-The temperature is more than or equal to 1700 ℃, and the calcium silicate board is not suitable for being used as an external heat-preservation and heat-insulation material. (2) The product has single size and is not suitable for heat preservation of special-shaped parts. Calcium silicate boards with different thicknesses all belong to straight board shapes, are not suitable for construction when meeting special-shaped areas such as corners, grooves and round outer walls during construction, and need to be cut to adapt to irregular kiln outlines, but the adoption of the mode can not ensure close contact with a kiln, so that loosening and falling of heat insulation materials are easily caused. (3) During the production process of the calcium silicate board, a large amount of energy is consumed for wet grinding of quartz sand and steam curing of a board blank, and the environmental resource is not saved. 4. The calcium silicate board has lower mechanical strength. Compared with a light refractory heat-insulating material, the calcium silicate board has lower mechanical property and is easy to break under external force. Therefore, a heat insulation material which can be used in a high-temperature environment of a kiln, has a light volume density and a small heat conductivity coefficient, and is convenient to construct and capable of adapting to various special-shaped parts of the kiln is urgently needed. At present, the industry personnel research and develop a heat insulation material, a porous light heat insulation refractory material and a preparation method thereof, the patent number is 200810225985.2, the heat insulation refractory material uses sawdust coke powder as a pore forming agent, and the density reaches 0.45g/cm3. The main crystal phases of the heat-insulating material are mullite and anorthite, the anorthite exists in the material, and the product is fired at 1500 ℃, so that the product can shrink greatly after being fired, holes in the material can shrink and deform due to the large shrinkage, the heat-insulating performance is reduced, a secondary processing procedure after being fired is required, and the product cannot be coated on site for construction of special-shaped parts, so that the use occasion of the material is limited. A refractory brick with superfine pores and high strength for insulating heat is prepared from high-alumina bauxite, floating bead, powdered coal ash and kaolin through preparing micropores by chemical foaming agent, and preparing high-alumina clay insulating material from high-alumina bauxite, floating bead, powdered coal ash and kaolin. Because the adopted raw materials contain various impurity elements such as Na2O、K2O、S、Fe2O3In which Fe2O3Up to a maximum of 2.5%, which has led to the fact that the invention cannot be used in high-temperature environmentsThe specification shows that the maximum use temperature of the material is 1400 ℃, in addition, the product is only suitable for being made into products, and the manufacturing process needs to prepare foam independently, so that the product is not suitable for direct use and field construction. The light heat-insulating pouring material is made up by using (patent No. 201110327920.0) water glass as binding agent, and contains more Na2O、K2O low-melting-point substances can generate more low-melting-point phases at high temperature, and the service performance of the material at high temperature is influenced.
Disclosure of Invention
In order to avoid the problems, the patent provides a fiber-reinforced high-temperature-resistant light high-alumina foaming coating material which adopts high-alumina bauxite powder, mullite powder, silicon micropowder, activated alumina micropowder, calcium aluminate cement, alumina sol, zirconium aluminate refractory cellucotton and an additive. The specific formula is as follows:
20-50% of high alumina bauxite powder,
50 to 80 percent of mullite powder
0 to 25 percent of silicon micropowder
0 to 10 percent of active alumina micro powder
25-55% of calcium aluminate cement
0 to 10 percent of aluminum sol
0.5 to 2.5 percent of additional zirconium aluminate refractory cellucotton
0.1 to 0.8 percent of sodium dodecyl benzene sulfonate foaming agent is added
0.05 to 0.22 percent of additional FDN-A water reducing agent
Sodium polyacrylate 0.05-0.35%
0.01 to 0.18 percent of citric acid is added
0.1 to 0.25 percent of external addition polycarboxylic acid water reducing agent
1.1 to 2.9 percent of carboxymethyl cellulose is added
35 to 45 percent of water is added into the mixture
Wherein the high-alumina bauxite powder has a required particle size diameter of 50-100 μm, and Al is contained in the raw material2O3More than or equal to 80, the mullite powder is a commercial product, the diameter of the finely ground particle is required to be 75-90 mu m, and the silicon micropowder is a commercial product, and the SiO is required to be2Not less than 99.8%, and d thereof50(50% of the size of the screen residue boundary) is less than or equal to 3 mu m, and the activated alumina micro powder is a commercial product, and d is50(50% of the size of the screen residue boundary) is less than or equal to 5 mu m, and the silicon micropowder is a commercial product and requires SiO2Not less than 94%, d thereof50(50% of the size of the screen residue boundary) is less than or equal to 3 mu m, the aluminum sol is a commercial product which is milky white liquid, the pH value is 5-6, the particle size of the sol is 10-15nm, and the solid content of the solvent is 20%. The zirconium aluminate refractory fiber cotton is a commercial product, and the fiber length is 2-5 mm.
High alumina bauxite powder or mullite powder, silica micropowder and active alumina are used as slurry raw materials, aluminate cement and alumina sol are used as binding agents, high-strength refractory fiber is used as a reinforcing blank, 35-45% of water is added to the raw materials, then sodium dodecyl benzene sulfonate foaming agent is added for rapid stirring, and the mixture can be directly smeared on the construction surface after the stirring is finished.
The invention has simple preparation process, saves the step of preparing foam in advance, is convenient to use immediately after being prepared on site during construction, and has the specific beneficial effects that:
(1) the material is composed of raw materials which generate mullite partially in situ, and because of high temperature, the material generates continuous mullite phase by in situ reaction, the high-temperature strength of the material is improved, the highest use temperature can reach 1420 ℃, and the linear shrinkage rate of the material after being fired at 1450 ℃ is within the range of +/-2.0%.
(2) The invention abandons the method of adding the heat-insulating aggregate into the traditional heat-insulating material, adopts the high-temperature refractory fiber to replace the lightweight aggregate, and has the compressive strength of 4-6 MPa; the slurry is foamed by adopting a chemical foaming agent, closed and fine air holes can be obtained after the slurry is foamed, the volume density and the heat conductivity coefficient of the material can be effectively reduced, and the material is measured by adopting a YB/T4130-2005 refractory material heat conductivity coefficient test methodThe thermal conductivity coefficient can reach 0.05-0.25 w/mk at 350 ℃, and the bulk density is 490kg/cm3Within the range.
(3) The invention adopts the calcium aluminate cement and the alumina sol as the binding agent, the calcium aluminate cement ensures that the thermal insulation coating material smeared on any surface can be quickly solidified within 30-65min to generate strength, and the construction time can be reasonably controlled.
(4) The alumina sol in the formula not only provides the drying strength of the sample, but also is converted into active alumina nano particles at high temperature and reacts with the silica micro powder in the raw material in situ, so that the combination of the mullite high-temperature phase of the sample is promoted, and the high-temperature combination strength of the sample can be further improved.
The invention can adapt to the construction of special-shaped areas of the kiln, such as corners, grooves and round outer walls, and avoids the phenomenon that the heat insulation material at the special-shaped part of the kiln is not tightly contacted with the kiln and falls off and loosens.
Detailed Description
Example 1
The raw materials are as follows: 40% of high-aluminA bauxite powder, 10% of silicon micropowder, 10% of active aluminA micropowder, 30% of calcium aluminate cement, 10% of aluminA sol, 1.5% of additional zirconium aluminate refractory cellucotton, 0.8% of additional sodium dodecyl benzene sulfonate foaming agent, 0.22% of FDN-A water reducing agent, 0.35% of additional sodium polyacrylate, 0.12% of additional citric acid, 0.25% of additional polycarboxylic acid water reducing agent, 2.5% of additional carboxymethyl cellulose and 45% of additional water, wherein the high-aluminA bauxite powder is required to have A particle size diameter of 50-120 mu m, and Al in the raw material is Al2O3Not less than 80, the activated alumina micropowder is a commercial product, and d is50(50% of the size of the screen residue boundary) is less than or equal to 5 mu m, and the silicon micropowder is a commercial product and requires SiO2Not less than 99.8%, and d thereof50(50% of the size of the screen residue boundary) is less than or equal to 3 mu m, the alumina sol is a commercial product which is a milky white liquid, the pH value is 6, the particle size of the sol is 10-15nm, the solid content of the solvent is 20%, the zirconium aluminate refractory fiber cotton is a commercial product, the short cut length of the fiber cotton is 2-5mm, the coating is filled into a fixed mold, the sample is cured for 28min and generates strength, and after curing, demolding and drying at 110 ℃ (24 hours), the sample is heated to 1400 ℃ and is kept warm for 3 hours to prepare the fired sample.
Example 2
45 percent of high-alumina bauxite powder
10 percent of silicon micropowder
5 percent of active alumina micro powder
5 percent of calcium aluminate cement
35 percent of aluminum sol
1.5 percent of additional zirconium aluminate refractory fiber cotton
0.8 percent of sodium dodecyl benzene sulfonate foaming agent is added
0.22 percent of additional FDN-A water reducing agent
0.35 percent of sodium polyacrylate
0.12 percent of citric acid is added
0.25 percent of external addition polycarboxylic acid water reducing agent
2.5 percent of carboxymethyl cellulose is added
Adding 45 percent of water into the mixture
Wherein the high-alumina bauxite powder has a required particle size diameter of 50-120 μm, and Al is contained in the raw material2O3Not less than 80, the activated alumina micropowder is a commercial product, and d is50(50% of the size of the screen residue boundary) is less than or equal to 5 mu m, and the silicon micropowder is a commercial product and requires SiO2Not less than 99.8%, and d thereof50(50% of the size of the screen residue boundary) is less than or equal to 3 mu m, the aluminum sol is a commercial product which is milky white liquid, the pH value is 6, the particle size of the sol is 10-15nm, and the solid content of the solvent is 20%. The zirconium aluminate refractory fiber cotton is a commercial product, and the fiber length is 2 mm. Filling the coating into a fixed mold, curing the sample within 45min to generate strength, curing, demolding, drying at 110 deg.C (24 hr), heating to 1400 deg.C, and maintaining for 3 hr to obtain the final product.
Example 3
60 percent of mullite micro powder
10 percent of silicon micropowder
Active alumina micropowder 8%
Clay fine powder 2%
20 percent of calcium aluminate cement
1.5 percent of additional zirconium aluminate refractory fiber cotton
0.5 percent of sodium dodecyl benzene sulfonate foaming agent is added
0.12 percent of additional FDN-A water reducing agent
0.15 percent of sodium polyacrylate
0.08 percent of citric acid is added
0.1 percent of external addition polycarboxylic acid water reducing agent
0.4 percent of carboxymethyl cellulose is added
42 percent of water is added outside
Wherein the mullite micropowder is a commercial commodity and is required to be finely ground to 50-120 μm, the silicon micropowder is a commercial commodity and is required to have SiO2 more than or equal to 99.8 percent and d50(50 percent of the size of the screen residue boundary) less than or equal to 3 μm, the activated alumina micropowder is a commercial commodity and has d50(50% of the size of the screen residue boundary) is less than or equal to 5 mu m, and the clay fine powder is a commercial product and is required to be finely ground to 180 meshes. The zirconium aluminate refractory fiber cotton is a commercial product, and the fiber length is 5 mm. Filling the coating material into a fixed mould, curing the sample for 29min, drying the cured sample at 110 ℃ (24 hours), heating to 1400 ℃ and preserving heat for 3 hours to obtain the fired sample.
Example 4
50 percent of mullite micro powder
8 percent of silicon micropowder
10 percent of active alumina micro powder
Clay fine powder 2%
30 percent of calcium aluminate cement
1.5 percent of additional zirconium aluminate refractory fiber cotton
0.7 percent of sodium dodecyl benzene sulfonate foaming agent is added
0.09 percent of additional FDN-A water reducing agent
0.15 percent of sodium polyacrylate
0.08 percent of citric acid is added
0.1 percent of external addition polycarboxylic acid water reducing agent
0.6 percent of carboxymethyl cellulose is added
40 percent of water is added outside
Wherein the mullite micropowder is a commercially available commodity and is required to be finely ground to 50-120 μm, and the silicon micropowder is a commercially available commodity and is required to have SiO2 of more than or equal to 99.8 percent and d of the SiO250(50% of the size of the screen residue boundary) is less than or equal to 3 mu m, and the activated alumina micro powder is a commercial product, and d is50(50% of the size of the screen residue boundary) is less than or equal to 5 mu m, and the clay fine powder is a commercial product and is required to be finely ground to 180 meshes. The zirconium aluminate refractory fiber cotton is a commercial product, and the fiber length is 2 mm. Filling the coating material into a fixed mould, curing the sample for 30min, curing the cured sample to generate strength, drying at 110 ℃ (24 hours), heating to 1400 ℃, and preserving heat for 3 hours to obtain the fired sample.
Example 5
Mullite micropowder 40%
18 percent of silicon micropowder
10 percent of active alumina micro powder
Clay fine powder 2%
5 percent of calcium aluminate cement
Aluminum sol 25%
1.5 percent of additional zirconium aluminate refractory fiber cotton
0.7 percent of sodium dodecyl benzene sulfonate foaming agent is added
0.07 percent of additional FDN-A water reducing agent
0.15 percent of sodium polyacrylate
0.08 percent of citric acid is added
0.1 percent of external addition polycarboxylic acid water reducing agent
0.6 percent of carboxymethyl cellulose is added
Adding 45 percent of water into the mixture
Wherein the mullite micropowder is a commercially available commodity and is required to be finely ground to 50-120 μm, and the silicon micropowder is a commercially available commodity and is required to have SiO2 of more than or equal to 99.8 percent and d of the SiO250(50% of the size of the screen residue boundary) is less than or equal to 3 mu m, the alumina sol is a commercial product which is milk white liquid with the pH value of 6, the particle size of the sol is 10-15nm, the solid phase content of the solvent is 20%, the activated alumina micropowder is a commercial product, and the d is the same as the active alumina micropowder50(50% of the size of the screen residue boundary) is less than or equal to 5 mu m, and the clay fine powder is a commercial product and is required to be finely ground to 180 meshes. The zirconium aluminate refractory fiber cotton is a commercial product, and the fiber length is 2 mm. Filling the coating into a fixed mold, curing the sample for 35min to generate strength, curing, demolding, drying at 110 ℃ (24 hours), heating to 1400 ℃, and keeping the temperature for 3 hours to obtain the fired sample.
Comparative example
Mixing industrial mullite powder with 10wt% of sweet potato powder, 0.6wt% of sodium polyacrylate and 0.5wt% of sodium hexametaphosphate, adding water, stirring to prepare slurry with the solid phase content of 62.5wt%, and performing ball milling for 10 hours to obtain stable slurry. Dripping 0.6wt% of triton X-100 of the mass of the slurryIn the slurry, after the slurry is uniformly stirred at a low speed, the slurry is stirred for 5 minutes at a rotating speed of 800 revolutions per minute, and a large amount of foam is generated in the slurry. The foam slurry was added to a mold and placed in an oven at 80 ℃ for 1 hour. After the heat preservation is finished, cooling to room temperature, then transferring into a 60 ℃ oven for drying for 12 hours, and finally drying in a 120 ℃ oven for 24 hours. And heating the dried blank to 500 ℃ at the speed of 1 ℃/min, preserving heat for 1 hour, heating to 1300 ℃ at the speed of 5 ℃/min, preserving heat for 2 hours, and preparing a sample.
| Performance index | Comparative example | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Bulk density (kg/m)3） | 578 | 350 | 380 | 393 | 420 | 460 |
| Normal temperature compressive strength (MaP) | ≥2.0 | ≥3.5 | ≥3.5 | ≥4.0 | ≥4.5 | ≥4.5 |
| Line change after 1400 ℃ burn (%) | ≤-4.0 | ≤-1.5 | ≤-1.5 | ≤-1.8 | ≤-2.0 | ≤-2.0 |
| Thermal conductivity (350 ℃ +/-25 ℃) w/mk | 0.18 | 0.08 | 0.09 | 0.14 | 0.15 | 0.17 |
| Maximum service temperature (. degree. C.) | 1300 | 1400 | 1400 | 1450 | 1450 | 1450 |
The comparative product refers to mullite heat-insulating and heat-preserving castable which is currently used in linings of kilns, thermal equipment, flues and smoke windows in industrial departments such as metallurgy, machinery, petrochemical industry, electric power, building materials and the like.
Claims (2)
1. The fiber-reinforced high-temperature-resistant light high-aluminum foaming coating material is characterized in that: the formula of the coating material in percentage by weight is as follows:
20 to 50 percent of high-alumina bauxite powder
0 to 10 percent of silicon micropowder
0 to 15 percent of active alumina micro powder
25-55% of calcium aluminate cement
0 to 10 percent of aluminum sol
0.5 to 2.5 percent of additional zirconium aluminate refractory cellucotton
0.1 to 0.8 percent of sodium dodecyl benzene sulfonate foaming agent is added
0.05 to 0.22 percent of additional FDN-A water reducing agent
Sodium polyacrylate 0.05-0.35%
0.01 to 0.18 percent of citric acid is added
0.1 to 0.25 percent of external addition polycarboxylic acid water reducing agent
1.1 to 2.9 percent of carboxymethyl cellulose is added
35 to 45 percent of water is added into the mixture
Wherein the high-alumina bauxite powder has a required particle size diameter of 50-120 μm, and Al is contained in the raw material2O3Not less than 80 percent, and the activated alumina micro powder is a commercial product, and d is50Not more than 5 μm, the silicon micropowder is a commercial product, and SiO is required2Not less than 94%, d thereof50Less than or equal to 3 microns, the alumina sol is a commercial product which is a milky white liquid, the pH value is 5-6, the particle size of the sol is 10-15nm, the solid phase content of the solvent is 20%, the zirconium aluminate refractory fiber is a commercial product, and the fiber length is 2-5 mm.
2. The process for manufacturing spread according to claim 1, wherein: high alumina bauxite powder, silicon micropowder and alumina micropowder are used as slurry raw materials, aluminate cement and alumina sol are used as a binding agent, refractory fiber cotton and an additive are added, 35-45% of water is added to the raw materials, then a sodium dodecyl benzene sulfonate foaming agent is added for rapid stirring, and the mixture can be directly smeared on a construction surface after the stirring is finished.
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| CN103951452A (en) * | 2014-05-06 | 2014-07-30 | 郑州大学 | Preparation method of microporous kyanite-based lightweight insulating refractory material |
| CN105110801A (en) * | 2015-07-20 | 2015-12-02 | 山东乐江建筑新材料有限公司 | Foamed lightweight refractory castable and preparation method thereof |
| CN108610069A (en) * | 2018-06-14 | 2018-10-02 | 玉和建设有限公司 | A kind of heat-insulated press-in material |
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| MX2015002365A (en) * | 2012-08-21 | 2015-09-24 | Stellar Materials Inc | Refractory composition and process for forming article therefrom. |
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| CN101792294A (en) * | 2010-03-30 | 2010-08-04 | 武汉钢铁(集团)公司 | Light thermal-shield refractory castable |
| CN103951452A (en) * | 2014-05-06 | 2014-07-30 | 郑州大学 | Preparation method of microporous kyanite-based lightweight insulating refractory material |
| CN105110801A (en) * | 2015-07-20 | 2015-12-02 | 山东乐江建筑新材料有限公司 | Foamed lightweight refractory castable and preparation method thereof |
| CN108610069A (en) * | 2018-06-14 | 2018-10-02 | 玉和建设有限公司 | A kind of heat-insulated press-in material |
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