CN115849883B - Corrosion-resistant corundum wear-resistant castable easy to mold and preparation method thereof - Google Patents

Corrosion-resistant corundum wear-resistant castable easy to mold and preparation method thereof Download PDF

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CN115849883B
CN115849883B CN202211658834.2A CN202211658834A CN115849883B CN 115849883 B CN115849883 B CN 115849883B CN 202211658834 A CN202211658834 A CN 202211658834A CN 115849883 B CN115849883 B CN 115849883B
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parts
aggregate
castable
mixing
corundum
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CN115849883A (en
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张晟
吴俊杰
范小康
李业清
乔学干
李豪
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Yixing Xingbei Refractory Insulation Engineering Co ltd
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Yixing Xingbei Refractory Insulation Engineering Co ltd
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Abstract

The invention provides an easily-formed corrosion-resistant corundum wear-resistant castable and a preparation method thereof, wherein the castable comprises the following components in parts by weight: 65-75 parts of aggregate, 14-18 parts of plate-shaped corundum fine powder, 10-14 parts of porous mullite, 6-15 parts of silicon carbide, 1-3 parts of silicon micropowder, 4-6 parts of bonding coagulant and 2-3 parts of water reducer; the preparation method comprises the following steps: s1, premixing aggregate, S2, premixing powder, S3 and casting molding, wherein S4 and post treatment are performed, the formed aggregate can better play a role in skeleton and support, and is favorable for casting molding, so that the strength of a product is improved, the filling property is enhanced through the addition of powder, the fluidity of the product is increased, the high temperature resistance is enhanced, the thermal stability and the thermal shock resistance of the castable are better improved through the addition of porous mullite, the corrosion resistance of the castable is improved through the addition of silicon carbide, the molding effect can be enhanced through the addition of a bonding coagulant, and the molding time is shortened.

Description

Corrosion-resistant corundum wear-resistant castable easy to mold and preparation method thereof
Technical Field
The invention relates to the technical field of corundum castable materials, in particular to an easily-formed corrosion-resistant corundum wear-resistant castable material and a preparation method thereof.
Background
The corundum has alpha-Al mineral phase 2 O 3 The refractory castable is characterized by high refractoriness, high mechanical strength and the like, is widely applied to industries such as metallurgy, building materials, petrochemical industry and the like, and is commonly used as lining materials of various kilns such as boilers, blast furnace hot blast stoves, heating furnaces, ceramic kilns and the like.
At present, the refractory product using corundum as main crystal phase is compounded by adding proper quantity of dispersing agent, coagulant and stainless steel fibre according to strict formula. Has good high-temperature strength, wear resistance, scouring resistance, high heat conduction and thermal shock resistance corrosion resistance, good sealing performance, quick setting and early strength, etc. The refractory castable is prepared by taking corundum as aggregate and adding some binding agents. Has higher mechanical strength and abrasion resistance than high-alumina refractory castable and mullite refractory castable, but has slightly poorer thermal shock resistance. The phosphoric acid binding agent is easy to react with iron mixed into refractory aggregate and powder during crushing to generate gas, so that the volume of the castable is expanded, and the mechanical property is reduced; the corundum castable material using corundum micropowder and alumina sol as binding agents has the problems of difficult molding, low strength after demolding, high construction difficulty, low demolding strength of a blank body, inconvenient construction and the like, and limits the application of the corundum castable material. The need for silica sol in combination with refractory castable is to find new gelling agents to shorten the curing time and improve the green mechanical strength without affecting the drying speed, so there is a strong need for binder-containing castable that can enhance the gelation effect and shorten the curing time.
Disclosure of Invention
In order to solve the technical problems, the invention provides an anti-corrosion corundum wear-resistant castable easy to mold and a preparation method thereof.
The technical scheme of the invention is as follows:
an anti-corrosion corundum wear-resistant castable easy to form comprises the following components in parts by weight: 65-75 parts of aggregate, 14-18 parts of plate-shaped corundum fine powder, 10-14 parts of porous mullite, 6-15 parts of silicon carbide, 1-3 parts of silicon micropowder, 4-6 parts of bonding coagulant and 2-3 parts of water reducer;
wherein the aggregate consists of plate-shaped corundum particles with the granularity of 2-7 mm, white corundum particles with the granularity of 2-5 mm and brown corundum particles with the granularity of 1-3 mm according to the weight ratio of 1-3: 1: mixing materials in a proportion of 1 to 3 to obtain; the bonding coagulant is prepared from polyvinyl alcohol, aluminum metaphosphate and magnesium silicate in a weight ratio of 1-3: 1:1 are mixed and prepared.
Description: through the proportion, the formed aggregate can better play a role in framework and support, is beneficial to casting molding, ensures proper volume density of the product, obviously improves the strength, enhances the filling property through the addition of powder, improves the construction property, thereby increasing the fluidity, enhancing the high temperature resistance, better improving the heat stability and the thermal shock resistance of the castable through the addition of porous mullite, improving the corrosion resistance of the castable through the addition of silicon carbide, enhancing the molding effect through the addition of a bonding coagulant, and shortening the molding time.
Further, the preparation method of the porous mullite comprises the following steps:
1) Taking mullite powder with the mass ratio of 0.1-0.3 mm, aluminum dihydrogen phosphate, aluminum sol and pore-forming agent as 3-5: 0.5:0.5:1, adding water with the same mass as the premix, stirring for 3-8 hours at the speed of 200-400 r/min, and preparing into pug;
2) Putting the pug trapped material obtained in the step 1) into a baking oven at 70-80 ℃ for 3-6 h until the pug trapped material is completely dried to form a green body;
3) And (3) placing the green body into a high-temperature muffle furnace, calcining, preserving heat, and crushing to obtain the porous mullite with the thickness of 0.05-0.25 mm.
Description: by the preparation method, the heat conductivity of the porous mullite can be effectively reduced, the problems of poor oxidation resistance and corrosion resistance of the existing porous mullite are solved, the structure and the molding effect of the mixed powder can be improved, and the porous mullite with higher air permeability and higher strength on the surface can be obtained by better combining the powder with a binder.
Further, the preparation method of the pore-forming agent in the step 1) comprises the following steps: rice hull powder, rosin resin, high-alumina minerals and water in the weight ratio of 8-12: 3:3: 15-25, fully soaking for 30-60 min under the condition of 5-8 kPa, then stirring for 2-4 h, and standing for 10min to obtain the pore-forming agent.
Description: the pore-forming agent prepared by the method uses rice hull powder as biomass powder for combustion and volatilization to generate pores, and the porosity is improved by the cooperation of high-alumina minerals and rosin resin; meanwhile, the uniformity of the porous mullite skeleton network structure is improved, and uniform and fine lap joint gaps are increased.
Further, the trapping conditions in the step 2) are as follows: placing for 3-6 h in a sealed environment with humidity of 40-60% and temperature of 60-65 ℃.
Description: through the above-mentioned stranded material condition, can make each component in the pug evenly distributed, improve pug's homogeneity and formability.
Further, the calcination heat preservation treatment in the step 3) is as follows: heating to 900-1000 ℃ at a heating rate of 8-10 ℃/min, preserving heat for 2h, heating to 1350-1600 ℃ at a heating rate of 3-5 ℃/min, preserving heat for 1-3 h, and cooling along with a furnace.
Description: the method can remove impurities and separate and enrich useful components, further increase the specific surface area of porous mullite and improve the pore structure.
Further, the water reducer is prepared from sulfonated acetonyl formaldehyde resin and aldehyde ketone 1: 1.
Description: through the use of the water reducer, the mud particles have a good dispersing effect, so that the workability of the mud particles can be improved, the unit water consumption is reduced, and the fluidity of the concrete mixture is improved.
Further, the granularity of the plate-shaped corundum fine powder and the silicon carbide is 2-5 mu m, and the granularity of the silicon micro powder is 0.5-1 mu m of SiO in the silicon micro powder 2 The content of the porous mullite is more than or equal to 90 percent, and the granularity of the porous mullite is 0.05 to 0.25mm.
Description: by using the raw materials, the raw materials can be better utilized to perform proportioning, so that better effects are generated on various performances of the castable.
A preparation method of an anti-corrosion corundum wear-resistant castable easy to form comprises the following steps:
s1, premixing aggregate:
mixing and stirring the aggregate and 50% of bonding coagulant for 10-15 min, wherein the mixing humidity is 70-75%, and the temperature is 1-5 ℃;
s2, premixing powder:
mixing and stirring plate-shaped corundum fine powder, porous mullite, silicon carbide, silicon micropowder, the rest 50% of bonding coagulant and water reducer for 3-5 min under the conditions of mixing humidity of 10-25% and room temperature;
s3, casting and forming:
adding water accounting for 2-4% of the mass of the aggregate into the pre-mixed aggregate obtained in the step S1, mixing and stirring for 3-5 min, adding the powder material premixed in the step S2, stirring for 5-10 min, adding water accounting for 8-10% of the mass of the aggregate, stirring for 10-15 min to obtain a wet mixed material, and pouring and vibrating the wet mixed material to obtain a pre-pouring material;
s4, post-treatment
And (3) curing, drying and heat treating the pre-cast material subjected to vibration molding in the step (S3) in sequence to obtain the cast material.
Description: through the preparation method, the bonding coagulant, the aggregate and the powder can be mixed more reasonably, the bonding effect is enhanced, the molding rate is improved, the wear resistance of the castable can be improved through mixed casting and post-treatment, the hardening speed can be further accelerated, the seepage resistance is improved, the corrosion of the phase interface between the raw materials is reduced, and the corrosion resistance is improved.
Further, the curing method in step S4 is as follows: and coating a layer of concrete water-saving moisture-preserving curing film on the surface of the pre-cast material, and curing for 2-6 h at the temperature of 20-30 ℃.
Description: the curing is performed by the method, so that the pre-cast material accelerates the hardening and forming and enhances the strength of the pre-cast material.
Further, the drying method in step S4 is as follows: drying the cured pre-cast material with hot air at 50-110 ℃ for 2-3 h, wherein the ventilation speed is 0.2-0.4 m/s; the heat treatment method comprises the following steps: heating the dried pre-cast material to 1000-1350 ℃ at a heating rate of 10 ℃/min, preserving heat for 1-4 h, heating while introducing ozone with an initial concentration of 15mg/L, increasing the ozone introducing amount at a speed of 1-5 mg/L every ten minutes, and reducing the ozone introducing amount to zero at a speed of 3-8 mg/L every ten minutes after starting heat preservation.
Description: the castable has relatively good thermal shock resistance through the treatment by the method; by introducing ozone, sintering of the material is promoted, a denser transition zone is formed between particles and a matrix, so that the structure is denser, the matrix and aggregate are better combined, and when the abrasion medium erodes the surface of the sample, the abrasion degree of the matrix and the aggregate is more uniform, thereby improving the abrasion resistance effect.
The beneficial effects of the invention are as follows:
(1) According to the invention, through the proportion of the raw material components, the formed aggregate can better play a role of a framework and a supporting function, and is beneficial to casting molding, so that the strength of a product is obviously improved, the filling property is enhanced through the addition of powder, the workability is improved, the fluidity is increased, the high temperature resistance is enhanced, the heat stability and the thermal shock resistance of the castable are better improved through the addition of porous mullite, the corrosion resistance of the castable is improved through the addition of silicon carbide, the molding effect can be enhanced through the addition of a bonding coagulant, and the molding time is shortened.
(2) According to the preparation method of the castable, the bonding coagulant, the aggregate and the powder can be mixed more reasonably, the bonding effect is enhanced, the molding rate is improved, the wear resistance of the castable can be improved through mixed casting and post-treatment, the hardening speed can be further accelerated, the seepage resistance is improved, the corrosion of the easily corroded phase interface among the raw materials is reduced, and the corrosion resistance is improved; through post-treatment, the castable can have relatively excellent thermal shock resistance; the sintering of the material is promoted, a denser transition zone is formed between particles and the matrix, so that the structure is denser, the matrix and aggregate are better combined, and when the abrasion medium erodes the surface of the sample, the abrasion degree of the matrix and the aggregate is more uniform, thereby improving the abrasion resistance effect.
(3) According to the preparation method of the porous mullite, the heat conductivity of the porous mullite can be effectively reduced, the problems of poor oxidation resistance and corrosion resistance of the conventional porous mullite are solved, the structure and the molding effect of mixed powder can be improved, and the porous mullite is better combined with a binder to obtain the porous mullite with higher air permeability and higher strength on the surface; the rice hull powder is used as biomass powder for combustion volatilization to generate air holes through the preparation of the pore-forming agent, and the porosity is improved through the cooperation of high-alumina minerals and rosin resin; meanwhile, the uniformity of the mullite porous skeleton network structure is improved, and uniform and fine lap joint gaps are increased; through the use of the water reducer, the cement mortar has a good dispersing effect on mud particles, can improve the workability, reduce the unit water consumption and improve the fluidity of the concrete mixture.
Detailed Description
The invention will be described in further detail with reference to the following embodiments to better embody the advantages of the invention.
Example 1
A preparation method of an anti-corrosion corundum wear-resistant castable easy to form comprises the following steps:
the weight portion comprises: 70 parts of aggregate, 15 parts of plate-shaped corundum fine powder, 13 parts of porous mullite, 10 parts of silicon carbide, 2 parts of silicon micropowder, 5 parts of bonding coagulant and 2.5 parts of water reducer; the porous mullite adopts the grain diameter of 0.05-0.25 mm sold in the market, and the corresponding amount of 100 parts is 1kg;
wherein the aggregate consists of plate-shaped corundum particles with the granularity of 2-7 mm, white corundum particles with the granularity of 2-5 mm and brown corundum particles with the granularity of 1-3 mm in a weight ratio of 2:1:2, mixing the materials in proportion to obtain the product;
the bonding coagulant consists of polyvinyl alcohol, aluminum metaphosphate and magnesium silicate in a weight ratio of 2:1:1, mixing and preparing;
the water reducer is prepared from sulfonated acetone formaldehyde resin and aldehyde ketone 1:1, preparing;
the granularity of the plate-shaped corundum fine powder and the silicon carbide is 2-5 mu m, and the granularity of the silicon micro powder is 0.5-1 mu m of SiO in the silicon micro powder 2 The content of (2) is more than or equal to 90%;
s1, premixing aggregate:
mixing and stirring the aggregate and 50% of bonding coagulant for 12min, wherein the mixing humidity is 72%, and the temperature is 2 ℃;
s2, premixing powder:
mixing and stirring plate-shaped corundum fine powder, porous mullite, silicon carbide, silicon micropowder, the rest 50% of bonding coagulant and water reducer for 4min under the conditions of mixing humidity of 15% and room temperature;
s3, casting and forming:
adding water accounting for 3% of the mass of the aggregate into the pre-mixed aggregate obtained in the step S1, mixing and stirring for 4min, adding the pre-mixed powder obtained in the step S2, stirring for 8min, adding water accounting for 9% of the mass of the aggregate, stirring for 12min to obtain a wet mixed material, and pouring and vibrating the wet mixed material to obtain a pre-pouring material;
s4, post-treatment
Curing, drying and heat treatment are sequentially carried out on the pre-cast material subjected to vibration molding in the step S3, so as to obtain a casting material; the maintenance method comprises the following steps: coating a layer of concrete water-saving moisture-preserving curing film on the surface of the pre-cast material, and curing for 4 hours at the temperature of 25 ℃; the water-saving and moisture-preserving curing film for concrete is commercially available.
Example 2
The embodiment is different from the embodiment 1 in that the raw material components are different, and the raw material components comprise the following components in parts by weight: 65 parts of aggregate, 18 parts of plate-shaped corundum fine powder, 14 parts of porous mullite, 6 parts of silicon carbide, 3 parts of silicon micropowder, 4 parts of bonding coagulant and 3 parts of water reducer;
wherein the aggregate consists of plate-shaped corundum particles with the granularity of 2-7 mm, white corundum particles with the granularity of 2-5 mm and brown corundum particles with the granularity of 1-3 mm in a weight ratio of 3:1:1, mixing the materials in proportion.
Example 3
The embodiment is different from the embodiment 1 in that the raw material components are different, and the raw material components comprise the following components in parts by weight: 75 parts of aggregate, 14 parts of plate-shaped corundum fine powder, 10 parts of porous mullite, 15 parts of silicon carbide, 1 part of silicon micropowder, 6 parts of bonding coagulant and 2 parts of water reducer;
wherein the aggregate consists of plate-shaped corundum particles with the granularity of 2-7 mm, white corundum particles with the granularity of 2-5 mm and brown corundum particles with the granularity of 1-3 mm in a weight ratio of 1:1:3, mixing the materials in proportion.
Example 4
The present example differs from example 1 in that the composition of the binding coagulant is different, and the binding coagulant is composed of polyvinyl alcohol, aluminum metaphosphate and magnesium silicate in a weight ratio of 1:1:1 are mixed and prepared.
Example 5
The present example differs from example 1 in that the composition of the binding coagulant is different, and the binding coagulant is composed of polyvinyl alcohol, aluminum metaphosphate and magnesium silicate in a weight ratio of 3:1:1 are mixed and prepared.
Example 6
The difference between this embodiment and embodiment 1 is that the premixing parameters in step S1 and step S2 are different, and S1 and aggregate are premixed: mixing and stirring the aggregate and one half of the bonding coagulant for 10min, wherein the mixing humidity is 70%, and the temperature is 5 ℃;
s2, premixing powder: mixing and stirring the plate-shaped corundum fine powder, porous mullite, silicon carbide, silicon micropowder, the rest half of binding coagulant and water reducer for 5min under the conditions of mixing humidity of 10% and room temperature.
Example 7
The difference between this embodiment and embodiment 1 is that the premixing parameters in step S1 and step S2 are different, and S1 and aggregate are premixed: mixing and stirring the aggregate and one half of the bonding coagulant for 15min, wherein the mixing humidity is 75%, and the temperature is 1 ℃;
s2, premixing powder: mixing and stirring the plate-shaped corundum fine powder, porous mullite, silicon carbide, silicon micropowder, the rest half of binding coagulant and water reducer for 3min under the conditions of mixing humidity of 25% and room temperature.
Example 8
The difference between this embodiment and embodiment 1 is that the processing parameters in step S3 and step S4 are different, and S3, casting molding: adding water accounting for 4% of the mass of the aggregate into the pre-mixed aggregate obtained in the step S1, mixing and stirring for 3min, adding the pre-mixed powder obtained in the step S2, stirring for 10min, adding water accounting for 8% of the mass of the aggregate, stirring for 15min to obtain a wet mixed material, and pouring and vibrating the wet mixed material to obtain a pre-pouring material;
s4, post-processing: curing, drying and heat treatment are sequentially carried out on the pre-cast material subjected to vibration molding in the step S3, so as to obtain a casting material; the maintenance method comprises the following steps: and coating a layer of concrete water-saving moisture-preserving curing film on the surface of the pre-cast material, and curing for 6 hours at the temperature of 20 ℃.
Example 9
The difference between this embodiment and embodiment 1 is that the processing parameters in step S3 and step S4 are different, and S3, casting molding: adding water accounting for 2% of the mass of the aggregate into the pre-mixed aggregate obtained in the step S1, mixing and stirring for 5min, adding the pre-mixed powder obtained in the step S2, stirring for 5min, adding water accounting for 10% of the mass of the aggregate, stirring for 10min to obtain a wet mixed material, and pouring and vibrating the wet mixed material to obtain a pre-pouring material;
s4, post-processing: curing, drying and heat treatment are sequentially carried out on the pre-cast material subjected to vibration molding in the step S3, so as to obtain a casting material; the maintenance method comprises the following steps: and coating a layer of concrete water-saving moisture-preserving curing film on the surface of the pre-cast material, and curing for 2 hours at the temperature of 30 ℃.
Example 10
This example differs from example 1 in that a method for preparing porous mullite is provided:
1) Taking mullite powder with the mass ratio of 0.1-0.3 mm, aluminum dihydrogen phosphate, aluminum sol and pore-forming agent as follows: 0.5:0.5:1, adding water with the same mass as the premix, stirring for 5 hours at the speed of 300r/min, and preparing into pug; the preparation method of the pore-forming agent comprises the following steps: rice hull powder, rosin resin, high-alumina minerals and water are mixed according to the weight ratio of 10:3:3:20, fully soaking for 45min under the condition of 6kPa, stirring for 3h, and standing for 10min to obtain a pore-forming agent;
2) Putting the pug obtained in the step 1) into a baking oven at 75 ℃ for 4 hours until the pug is completely dried to form a green body; the material trapping conditions are as follows: placing in a sealed environment with humidity of 50% and temperature of 63 ℃;
3) Placing the green body into a high-temperature muffle furnace, calcining, preserving heat, and crushing to obtain 0.05-0.25 mm porous mullite; the calcination heat preservation treatment is as follows: heating to 950 ℃ at a heating rate of 9 ℃/min, preserving heat for 2 hours, heating to 1550 ℃ at a heating rate of 4 ℃/min, preserving heat for 2 hours, and cooling with a furnace.
Example 11
The embodiment is different from embodiment 10 in that the raw material composition ratio in step 1) is different, 1) mullite powder with the mass ratio of 0.1-0.3 mm is taken, aluminum dihydrogen phosphate, aluminum sol and pore-forming agent are taken as follows, and the mass ratio is 5:0.5:0.5:1, adding water with the same mass as the premix, stirring for 3 hours at the speed of 200r/min, and preparing into pug; the preparation method of the pore-forming agent comprises the following steps: rice hull powder, rosin resin, high-alumina minerals and water are mixed according to the weight ratio of 8:3:3:25, fully soaking for 30min under the condition of 5kPa, stirring for 4h, and standing for 10min to obtain the pore-forming agent.
Example 12
The embodiment is different from embodiment 10 in that the raw material composition ratio in step 1) is different, 1) mullite powder with the mass ratio of 0.1-0.3 mm is taken, aluminum dihydrogen phosphate, aluminum sol and pore-forming agent are mixed according to the mass ratio of 3:0.5:0.5:1, adding water with the same mass as the premix, stirring for 8 hours at the speed of 400r/min, and preparing into pug; the preparation method of the pore-forming agent comprises the following steps: rice hull powder, rosin resin, high-alumina minerals and water are mixed according to the weight ratio of 12:3:3:15, fully soaking for 60min under the condition of 8kPa, stirring for 2h, and standing for 10min to obtain the pore-forming agent.
Example 13
The difference between this example and example 10 is that the condition parameters in step 2) are different, 2) the pug obtained in step 1) is trapped for 6 hours, and put into a 70 ℃ oven to be dried completely, forming a green body; the material trapping condition is that the material is placed in a sealed environment with humidity of 40% and temperature of 60 ℃.
Example 14
The difference between this example and example 10 is that the condition parameters in step 2) are different, 2) the pug obtained in step 1) is trapped for 3 hours, and put into an oven at 80 ℃ to be dried completely, forming a green body; the material trapping condition is that the material is placed in a sealed environment with the humidity of 60 percent and the temperature of 65 ℃.
Example 15
The present example differs from example 10 in that the calcination heat preservation parameters in step 3) are different, the temperature is kept for 2 hours at a temperature rise rate of 8 ℃/min to 900 ℃, then the temperature is raised to 1350 ℃ at 5 ℃/min, and the temperature is kept for 3 hours, and then the furnace is cooled.
Example 16
The present example differs from example 10 in that the calcination heat preservation parameters in step 3) are different, the temperature is kept for 2 hours at a temperature rise rate of 10 ℃/min to 1000 ℃, then the temperature is raised to 1600 ℃ at 3 ℃/min, the temperature is kept for 1 hour, and then the furnace is cooled.
Example 17
The difference between this embodiment and embodiment 10 is that the drying method in step S4 is:
drying the cured pre-cast material with hot air at 80 ℃ for 2.5 hours, wherein the ventilation speed is 0.3m/s; the heat treatment method comprises the following steps: heating the dried pre-cast material to 1300 ℃ at a heating rate of 10 ℃/min, preserving heat for 3 hours, introducing ozone with an initial concentration of 15mg/L while heating, increasing the ozone introducing amount at a speed of 3mg/L every ten minutes, and reducing the ozone introducing amount to zero at a speed of 5mg/L every ten minutes after starting heat preservation;
example 18
The difference between this example and example 17 is that the drying and heat treatment parameters in step S4 are different, the pre-cast material after maintenance is dried by hot air at 110 ℃ for 2 hours, and the ventilation speed is 0.2m/S; and the temperature parameters in the heat treatment are that the temperature of the pre-cast material after drying is raised to 1000 ℃ and the temperature is kept for 4 hours.
Example 19
The difference between this example and example 17 is that the drying and heat treatment parameters in step S4 are different, the pre-cast material after maintenance is dried by hot air at 50 ℃ for 3 hours, and the ventilation speed is 0.4m/S; and the temperature parameters in the heat treatment are that the temperature of the pre-cast material after drying is raised to 1350 ℃ and the temperature is kept for 1h.
Example 20
This example is different from example 17 in that the ozone increasing rate is different, ozone having an initial concentration of 15mg/L is introduced while the temperature is raised, and the ozone introducing amount is increased at a rate of 1mg/L per ten minutes, and when the ozone introducing amount after the start of the heat preservation is reduced to zero at a rate of 3mg/L per ten minutes.
Example 21
This example is different from example 17 in that the ozone increasing rate is different, ozone having an initial concentration of 15mg/L is introduced while the temperature is raised, and the ozone introducing amount is increased at a rate of 5mg/L per ten minutes, and when the ozone introducing amount after the start of the heat preservation is reduced to zero at a rate of 8mg/L per ten minutes.
Experimental example
The experimental results are as follows:
1. the casting material molded products obtained in examples 1 to 3, 10 and 17 were each subjected to a weight loss amount test after 24 hours of immersing in 10% sulfuric acid and 10% sodium hydroxide, respectively, and the test results were as follows:
1. exploring the influence of different castable raw material components on the required setting time result;
comparative example 1: 70 parts of aggregate, 15 parts of plate-shaped corundum fine powder, 13 parts of porous mullite, 10 parts of silicon carbide, 2 parts of silicon micropowder and 2.5 parts of water reducer are arranged, a bonding coagulant is not added, and the rest of treatment is the same as that of example 1;
example 1 and example 2 were compared with example 3 and comparative example 1, as shown in table 1;
TABLE 1 results of Performance experiments on castable under different castable raw material compositions
As can be seen from table 1, the castable of example 1, example 10 and example 17 has better properties, and the components of example 1, example 2 and example 3 are optimally mixed, and the porous mullite of example 10 is adopted in comparative example 1 and example 10, so that the performances of the castable are improved, wherein the degree of improvement of compressive strength is larger; comparing example 10 with example 17, it can be seen that the castable properties are better after the treatment by the method of example 17; as can be seen from comparative examples 1 and 1, the adhesive coagulant has an influence on not only the setting time but also various properties of the castable, and example 17 is preferable in view of the combination.
2. The castable molded products obtained in examples 1 to 21 were each subjected to abrasion resistance and weight loss amount test after 24 hours of immersion in sulfuric acid having a concentration of 10%, and the test results were as follows:
2. the influence of different bonding coagulant components on the performance of the castable is explored;
example 1, example 4 and example 5 were taken for comparison as shown in table 2;
TABLE 2 castable Performance test results at different bond coagulant compositions
As can be seen from table 2, comparative examples 1, 4 and 5, it was found that the cohesive setting agent raw material component of example 1 was more preferable.
3. Exploring the influence of different treatment parameters on the performance of the castable;
examples 6 to 9 were taken for comparison as shown in Table 3;
TABLE 3 castable performance test results obtained with different treatment parameters
As can be seen from table 3, the premixing parameters of example 1, example 6 and example 7 were found to be preferable, and the mixing and post-treatment parameters of example 1, example 8 and example 9 were found to be preferable.
4. The influence of different porous mullite raw material components on the performance of the castable is explored;
examples 10 to 14 were taken for comparison as shown in Table 4;
TABLE 4 castable performance test results for different porous mullite raw material compositions
As can be seen from table 4, in comparative examples 10, 11 and 12, porous mullite obtained by proportioning the raw materials in example 10 is superior in the performance of the prepared castable, and in comparative examples 10, 13 and 14, the parameters set in example 10 are superior.
5. The influence of the temperature in the preparation of different porous mullite on the performance of the castable is explored;
comparative example 2: setting a heating rate of 8 ℃/min to 1350 ℃ in the step 3) of preparing porous mullite, and carrying out treatment by a calcination heat preservation treatment method of preserving heat for 2 hours, wherein the rest treatment is the same as that of the example 10;
examples 15 to 19 and comparative example 2 were compared with each other, as shown in Table 5;
TABLE 5 results of temperature vs. castable Performance experiments in the preparation of different porous mullite
As can be seen from table 5, comparing examples 10, 15 and 16, it can be seen that the calcination heat preservation parameters of example 10 are superior; comparative example 10 and comparative example 2, it can be seen that the calcination heat preservation method of example 10 is more preferable.
6. The influence of different drying and heat treatment methods on the performance of the castable is explored;
comparative example 3: setting ozone with constant concentration of 35mg/L in the step S4, and introducing until the heat preservation is finished; the rest of the treatment was the same as in example 17;
examples 17 to 21 and comparative example 3 were compared with each other, as shown in Table 6;
TABLE 6 results of performance experiments of different drying and heat treatment methods on castable
As can be seen from table 6, the castable prepared by the drying heat treatment method of example 17 has better performance as compared with examples 17, 18 and 19; comparative example 17, example 20 and example 21, comparative example 3, it can be seen that the heat treatment method of example 17 is optimal.

Claims (4)

1. The anti-corrosion corundum wear-resistant castable is characterized by comprising, by weight, 65-75 parts of aggregate, 14-18 parts of platy corundum fine powder, 10-14 parts of porous mullite, 6-15 parts of silicon carbide, 1-3 parts of silicon micropowder, 4-6 parts of binding coagulant and 2-3 parts of water reducer;
wherein the aggregate comprises plate-shaped corundum particles with the granularity of 2-7 mm, white corundum particles with the granularity of 2-5 mm and brown corundum particles with the granularity of 1-3 mm in a weight ratio of 1-3: 1: mixing materials in a proportion of 1-3 to obtain; the bonding coagulant is prepared from polyvinyl alcohol, aluminum metaphosphate and magnesium silicate in a weight ratio of 1-3: 1:1, mixing and preparing;
the preparation method of the porous mullite comprises the following steps:
1) Taking mullite powder with the mass ratio of 0.1-0.3 mm, aluminum dihydrogen phosphate, aluminum sol and pore-forming agent as 3-5: 0.5:0.5:1, mixing to form a premix, adding water with the same mass as the premix, stirring for 3-8 hours at the speed of 200-400 r/min, and preparing a pug; the preparation method of the pore-forming agent comprises the following steps: rice hull powder, rosin resin, high-alumina minerals and water in a weight ratio of 8-12: 3:3: mixing the materials according to the proportion of 15-25, fully soaking the materials for 30-60 min under the condition of 5-8 kPa, stirring the materials for 2-4 h, and standing the materials for 10min to obtain a pore-forming agent;
2) Placing the pug trapped material obtained in the step 1) into a baking oven at 70-80 ℃ for 3-6 hours until the pug trapped material is completely dried to form a green body;
3) Placing the green body into a high-temperature muffle furnace, calcining, preserving heat, and crushing to obtain 0.05-0.25 mm porous mullite; the calcination heat preservation treatment is as follows: heating to 900-1000 ℃ at a heating rate of 8-10 ℃/min, preserving heat for 2h, heating to 1350-1600 ℃ at a heating rate of 3-5 ℃/min, preserving heat for 1-3 h, and cooling along with a furnace;
the preparation method of the anti-corrosion corundum wear-resistant castable easy to form comprises the following steps:
s1, premixing aggregate:
mixing and stirring the aggregate and 50% of bonding coagulant for 10-15 min, wherein the mixing humidity is 70-75%, and the temperature is 1-5 ℃;
s2, premixing powder:
mixing and stirring plate-shaped corundum fine powder, porous mullite, silicon carbide, silicon micropowder, the rest 50% of bonding coagulant and a water reducing agent for 3-5 min under the conditions of mixing humidity of 10-25% and room temperature;
s3, casting and forming:
adding water accounting for 2-4% of the mass of the aggregate into the pre-mixed aggregate obtained in the step S1, mixing and stirring for 3-5 min, adding the powder obtained in the pre-mixing in the step S2, stirring for 5-10 min, adding water accounting for 8-10% of the mass of the aggregate, stirring for 10-15 min to obtain a wet mixed material, and pouring and vibrating the wet mixed material to obtain a pre-pouring material;
s4, post-treatment
Curing, drying and heat treatment are sequentially carried out on the pre-cast material subjected to vibration molding in the step S3, so as to obtain a casting material; the drying method comprises the following steps: drying the cured pre-cast material with hot air at 50-110 ℃ for 2-3 hours, wherein the ventilation speed is 0.2-0.4 m/s; the heat treatment method comprises the following steps: heating the dried pre-cast material to 1000-1350 ℃ at a heating rate of 10 ℃/min, preserving heat for 1-4 h, heating while introducing ozone with an initial concentration of 15mg/L, increasing the ozone introducing amount at a speed of 1-5 mg/L per ten minutes, and reducing the ozone introducing amount to zero at a speed of 3-8 mg/L per ten minutes after starting heat preservation; the water reducer is prepared from sulfonated acetone formaldehyde resin and aldehyde ketone 1: 1.
2. An easily formable corrosion resistant corundum wear resistant castable as claimed in claim 1, wherein the conditions of the material trapped in step 2) are: and placing the mixture for 3-6 hours in a sealed environment with the humidity of 40-60% and the temperature of 60-65 ℃.
3. The easily-formed corrosion-resistant corundum wear-resistant castable material as claimed in claim 1, wherein the plate-shaped corundum fine powder and silicon carbide are 2-5 μm in granularity, the silicon fine powder is 0.5-1 μm in granularity, and SiO in the silicon fine powder is as follows 2 The content of the porous mullite is more than or equal to 90 percent, and the granularity of the porous mullite is 0.05-0.25 mm.
4. The easily-formed corrosion-resistant corundum wear-resistant castable in accordance with claim 1, wherein the curing method in step S4 is as follows: and wrapping a layer of concrete water-saving moisture-preserving curing film on the surface of the pre-cast material, and curing for 2-6 hours at the temperature of 20-30 ℃.
CN202211658834.2A 2022-12-22 2022-12-22 Corrosion-resistant corundum wear-resistant castable easy to mold and preparation method thereof Active CN115849883B (en)

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Publication number Priority date Publication date Assignee Title
CN101671172A (en) * 2009-10-23 2010-03-17 中南大学 Composite binder for preparing sintered porous body of silicon carbide powder and using method thereof
CN106977216A (en) * 2017-04-05 2017-07-25 洛阳理工学院 Anti-erosion liner for aluminium melting furnace and preparation method thereof
CN110963807A (en) * 2019-11-28 2020-04-07 浙江锦诚新材料股份有限公司 Energy-saving mullite refractory brick for cement kiln transition zone and preparation method thereof
CN112608057A (en) * 2020-07-21 2021-04-06 科之杰新材料集团河南有限公司 Water reducing agent and preparation method thereof
CN113912414A (en) * 2021-10-28 2022-01-11 韶关学院 Method for preparing mullite porous heat-insulating material by using coal gangue

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EP1953125A4 (en) * 2005-10-27 2010-05-05 Nippon Steel Corp Monolithic refractory

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101671172A (en) * 2009-10-23 2010-03-17 中南大学 Composite binder for preparing sintered porous body of silicon carbide powder and using method thereof
CN106977216A (en) * 2017-04-05 2017-07-25 洛阳理工学院 Anti-erosion liner for aluminium melting furnace and preparation method thereof
CN110963807A (en) * 2019-11-28 2020-04-07 浙江锦诚新材料股份有限公司 Energy-saving mullite refractory brick for cement kiln transition zone and preparation method thereof
CN112608057A (en) * 2020-07-21 2021-04-06 科之杰新材料集团河南有限公司 Water reducing agent and preparation method thereof
CN113912414A (en) * 2021-10-28 2022-01-11 韶关学院 Method for preparing mullite porous heat-insulating material by using coal gangue

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