CN111943716A - Preparation method of novel red mud-fly ash based gradient structure porous ceramic - Google Patents
Preparation method of novel red mud-fly ash based gradient structure porous ceramic Download PDFInfo
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Abstract
The invention discloses a preparation method of novel red mud-fly ash based gradient structure porous ceramic, which comprises the following steps: pretreating red mud and fly ash: crushing red mud blocks, drying and sieving to obtain red mud, wherein the fly ash is first-grade ash; and (3) uniformly mixing powder: mixing the screened red mud, the screened fly ash and a foaming agent to obtain a porous ceramic powder raw material; pressing to form a blank and foaming: carrying out compression molding on the porous ceramic powder raw material to obtain a high-temperature pre-foamed blank, drying the blank at a drying temperature, carrying out high-temperature foaming and heat preservation to prepare porous ceramic with uniform plane aperture and gradient structural hole arrangement on a vertical section; according to the invention, by controlling the process, the porous ceramic with uniform planar pore size distribution and obvious gradient structure distribution of pores in the vertical section direction can be prepared without using a die and a special treatment means.
Description
Technical Field
The invention relates to the technical field of porous ceramic preparation, in particular to a preparation method of novel red mud-fly ash-based gradient structure porous ceramic.
Background
The preparation of the porous ceramic by utilizing industrial solid wastes has great significance for environmental protection and resource reutilization. The red mud is used as red powdery strong base solid waste generated by extracting aluminum oxide in the aluminum production industry, and generates huge stockpiling quantity every year, thereby not only polluting the environment, but also causing resource waste; the fly ash is used as solid waste produced by a thermal power plant and has high recycling value. The red mud and the fly ash both contain SiO2、Al2O3、Fe2O3CaO and the like, and the porous ceramic is prepared by the synergistic and complementary utilization of the red mud and the fly ash according to different physicochemical properties.
At present, more methods are used for preparing the porous ceramics. The traditional methods comprise a particle stacking forming method, a pore-forming agent adding method, a foaming pore-forming agent method, an organic precursor impregnation method, a solid sintering method, a sol-gel method and the like, wherein some preparation methods have large workload and have more requirements on raw materials and instruments, but only the foaming method is a mature method for preparing closed-pore ceramics at present; in addition, there are also known a freeze drying method, a bio-templating method, a gel injection molding method, a self-propagating high-temperature synthesis method, and the like, which are relatively novel. Dispersing agents and binding agents are required to be added into raw materials of a freeze drying method, slurry solid mold forming and vacuum drying are involved in the preparation process, and the processes are multiple and complex; and the other emerging processes have fine requirements on raw materials and preparation processes, and need special surfactants or compound templates. In the preparation process of the foaming method, people such as Liutao surge and the like use lead-zinc tailings, red mud and silica sand as main components, and Na2B4O7As fluxing agent, prepared at 900-1000 deg.CA high porosity ceramic foam with microscopic observation of a large number of closed cells, but different foaming mechanisms in the foaming result in a random distribution of a large number of closed cells of different pore sizes, which is also the predominant pore type structure of the porous ceramics seen today. The problem of single heat conductivity of the porous ceramic as a heat insulation material is solved by random bubble distribution, and if the bubbles are arranged according to a certain rule, different heat conductivities of different surfaces of the porous ceramic, which are in contact with the environment, can be realized, so that the field with special requirements on heat insulation and heat preservation is satisfied.
In view of the above-mentioned drawbacks, the inventors of the present invention have finally obtained the present invention through a long period of research and practice.
Disclosure of Invention
In order to solve the technical defects, the invention adopts the technical scheme that the method for preparing the novel porous ceramic with the gradient structure by utilizing the red mud-fly ash comprises the following steps:
s1, pretreating red mud and fly ash: crushing red mud blocks, drying and sieving to obtain red mud, wherein the fly ash is first-grade ash;
s2, mixing the powder: mixing the screened red mud, the screened fly ash and a foaming agent to obtain a porous ceramic powder raw material;
s3, pressing into a blank and foaming: and (2) carrying out compression molding on the porous ceramic powder raw material to obtain a high-temperature pre-foamed blank, drying the blank at a drying temperature, carrying out high-temperature foaming and heat preservation to obtain the porous ceramic with uniform plane aperture and gradient structural hole arrangement on a vertical section.
Preferably, in the step S1, the red mud blocks are crushed in a crusher for 1min to 5min, and are dried at 100 ℃ for 12h and then screened, and the red mud is obtained after being completely screened, wherein the granularity of the red mud is 100 meshes to 400 meshes.
Preferably, in the step S2, the red mud with a mass fraction of 50% to 90% and the fly ash with a mass fraction of 10% to 50% are mixed, and the addition amount of the foaming agent is 0.5 wt% to 1.5 wt%.
Preferably, the foaming agent is one or a mixture of more of silicon carbide, calcium carbonate, fluorite, calcium sulfate and manganese dioxide.
Preferably, in the step S2, the mixing time of the red mud, the fly ash and the foaming agent in the mixer is 1 to 3 hours.
Preferably, in the step S3, the pressure when the porous ceramic powder raw material is pressed is 50MPa to 300MPa, the drying temperature of the green body is 100 ℃ to 140 ℃, and the drying time is 6h to 12 h.
Preferably, the temperature in the high-temperature foaming process in step S3 is controlled as follows: when the current temperature is lower than 300 ℃, the heating rate is 4-8 ℃/min; keeping the temperature for 20-60 min when the current temperature is 300 ℃; when the current temperature is higher than 300 ℃, the heating rate is 3 ℃/min-5 ℃/min until the foaming temperature is reached, and the temperature is kept, wherein the foaming temperature is 1220-1280 ℃, and the temperature is kept for 30 min-90 min.
Compared with the prior art, the invention has the beneficial effects that: 1, except for the foaming agent, the raw materials used in the invention are completely industrial solid wastes, so that the production cost is greatly reduced, the pollution is reduced, and the method has important significance for environmental protection; 2, the method is simple to operate and low in cost, and the addition and treatment of other auxiliary materials are reduced in the preparation process, so that the complexity of the production process is reduced; 3, by controlling the process, the porous ceramic with uniform planar pore size distribution and obvious gradient structure distribution of pores in the vertical section direction can be prepared without using a die and a special treatment means; 4, the foaming temperature rise program is simple, safe and reliable, and the pore distribution of the prepared porous ceramic gradient structure is obviously different from that of the general porous ceramic.
Drawings
FIG. 1 is an XRD pattern of raw red mud;
FIG. 2 is an XRD pattern of a raw fly ash;
FIG. 3 is a schematic vertical sectional view of the porous ceramic prepared in the example;
FIG. 4 is a diagram showing the distribution of pores in the planar direction of the prepared porous ceramic.
Detailed Description
The above and further features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
The invention discloses a method for preparing novel porous ceramic with a gradient structure by utilizing red mud-fly ash, which comprises the following steps:
s1, pretreating red mud and fly ash: crushing red mud blocks in a solid sample crusher for a certain time, drying and sieving to obtain red mud, wherein the fly ash is first-grade ash;
s2, mixing the powder: mixing the screened red mud, the screened fly ash and a foaming agent according to a certain proportion, and mixing for a period of time in a mixer to obtain a raw material for preparing porous ceramic powder;
s3, pressing into a blank and foaming: and (2) carrying out compression molding on the porous ceramic powder raw material to obtain a high-temperature pre-foamed blank, drying the blank at a certain temperature for a period of time, then placing the blank into a high-temperature furnace to carry out high-temperature foaming by controlling a temperature rise program, and carrying out heat preservation for a period of time to obtain the porous ceramic with uniform plane aperture and gradient structural hole arrangement on the vertical section.
In the step S1, the red mud blocks are crushed in a solid crusher for 1min to 5min, and are dried at 100 ℃ for 12h and then screened, and the red mud particles with a particle size of 100 to 400 meshes are obtained after complete screening.
In the step S2, the red mud and the fly ash are mixed according to the mass fractions of 50% to 90% and 10% to 50%, respectively, the addition amount of the foaming agent is 0.5 wt% to 1.5 wt%, and the foaming agent is one or a mixture of more of silicon carbide, calcium carbonate, fluorite, calcium sulfate, manganese dioxide, and the like.
In the step S2, the proportioned raw materials are fully and uniformly mixed in a mixer for 1 to 3 hours.
In the step S3, the pressure when the porous ceramic powder raw material is pressed is 50 MPa-300 MPa, the drying temperature of the green body is 100 ℃ to 140 ℃, and the time is controlled to be 6 h-12 h, so as to remove the moisture in the sample and reduce the influence on foaming.
The temperature raising program control in step S3 is as follows: when the current temperature is lower than 300 ℃, the heating rate is 4 ℃/min to 8 ℃/min, and the temperature is kept at 300 ℃ for 20min to 60 min; when the current temperature is higher than 300 ℃, the heating rate is 3 ℃/min-5 ℃/min, the foaming temperature is 1220-1280 ℃, and the temperature is kept for 30 min-90 min.
As shown in fig. 1 and 2, fig. 1 is an XRD pattern of raw red mud; FIG. 2 is an XRD pattern of a raw fly ash; the XRD chart shows that the main components contained in the raw material red mud and the raw material fly ash provide feasibility for preparing the porous ceramic.
In the invention, except for the foaming agent, the used raw materials are completely industrial solid wastes, so that the production cost is greatly reduced, the pollution is reduced, and the method has important significance for environmental protection; the preparation method is simple to operate and low in cost, the addition and treatment of other auxiliary materials are reduced in the preparation process, and the complexity of the production process is reduced; according to the invention, by controlling the process, reasonably optimizing the ingredients and the process parameters, the porous ceramic with uniform planar pore size distribution and obvious gradient structure distribution of pores in the vertical section direction can be prepared without using a die and a special treatment means; the foaming temperature-rising program is simple, safe and reliable, and the prepared porous ceramic has a gradient structure and obvious hole distribution difference with common porous ceramic.
Example one
Pretreatment and batching of raw materials: crushing red mud to enable the particle size of the red mud to reach 100 meshes, drying the red mud and the fly ash at 100 ℃ for 12 hours, and mixing the red mud and the fly ash in a mixer for 1 hour, wherein the adding amount of the red mud is 88.65 wt%, the adding amount of the fly ash is 9.85 wt%, and the adding amount of a foaming agent is 1.5 wt%;
pressing to form a blank and processing: pressing the uniformly mixed pre-foamed powder raw materials into a cylindrical blank body with the diameter of 20 multiplied by 5mm under the pressure of 50MPa for 60s, and placing the demolded blank body into a drying oven for processing for 6h at the temperature of 140 ℃;
foaming procedure and temperature reduction: and (3) putting the dried green body into a mullite box body, heating the green body to 1220 ℃ in a high-temperature furnace, and preserving the temperature for 30min to obtain the novel red mud-fly ash porous ceramic, wherein the holes are distributed in the vertical section direction to form a gradient structure.
Example two
Pretreatment and batching of raw materials: crushing red mud to enable the particle size of the red mud to reach 150 meshes, drying the red mud and the fly ash at 100 ℃ for 12 hours, and uniformly mixing the red mud and the fly ash in a mixer for 1.5 hours, wherein the adding amount of the red mud is 78.8 wt%, the adding amount of the fly ash is 19.7 wt% and the adding amount of a foaming agent is 1.5 wt%;
pressing to form a blank and processing: pressing the uniformly mixed pre-foamed powder raw materials into a cylindrical blank body with the diameter of 20 multiplied by 5mm under the pressure of 125MPa for 60s, and drying the demolded blank body in a drying oven at the temperature of 130 ℃ for 8 h;
foaming procedure and temperature reduction: and (3) putting the dried sample into a mullite box, heating to 1240 ℃ in a high-temperature furnace, and keeping the temperature for 40min to obtain the novel red mud-fly ash porous ceramic, wherein the holes are distributed in the vertical section direction to form a gradient structure, and the real object is shown in fig. 3 (a).
EXAMPLE III
Pretreatment and batching of raw materials: crushing red mud to enable the particle size of the red mud to reach 200 meshes, drying the red mud and the fly ash at 100 ℃ for 12 hours, and uniformly mixing the red mud and the fly ash in a mixer for 2 hours, wherein the adding amount of the red mud is 69.3 wt%, the adding amount of the fly ash is 29.7 wt% and the adding amount of a foaming agent is 1.0 wt%;
pressing to form a blank and processing: pressing the uniformly mixed pre-foaming powder raw materials into a cylindrical blank body with the diameter of 20 multiplied by 5mm under the pressure of 175MPa for 90s, and drying the demoulded blank body in a drying oven at the temperature of 120 ℃ for 10 h;
foaming procedure and temperature reduction: and putting the dried sample into a mullite box, heating to 1260 ℃ in a high-temperature furnace, and keeping the temperature for 50min to obtain the novel red mud-fly ash porous ceramic, wherein the pores are distributed in the vertical section direction to form a gradient structure.
Example four
Pretreatment and batching of raw materials: crushing red mud to enable the particle size of the red mud to reach 300 meshes, drying the red mud and the fly ash at 100 ℃ for 12 hours, and uniformly mixing the red mud and the fly ash in a mixer for 2.5 hours, wherein the adding amount of the red mud is 59.4 wt%, the adding amount of the fly ash is 39.6 wt% and the adding amount of a foaming agent is 1.0 wt%;
pressing to form a blank and processing: keeping the pressure of the uniformly mixed pre-foaming powder raw materials for 120s under 225MPa, pressing the uniformly mixed pre-foaming powder raw materials into a cylindrical blank with the diameter of 20 multiplied by 5mm, and drying the demolded blank in a drying oven at the temperature of 110 ℃ for 10 hours;
foaming procedure and temperature reduction: and (3) putting the dried sample into a mullite box, heating the sample to 1270 ℃ in a high-temperature furnace, and keeping the temperature for 60min to obtain the novel red mud-fly ash porous ceramic, wherein the pores are distributed in the vertical section direction to form a gradient structure, and the real object is shown in fig. 3 (b).
EXAMPLE five
Pretreatment and batching of raw materials: crushing red mud to enable the particle size of the red mud to reach 400 meshes, drying the red mud and the fly ash at 100 ℃ for 12 hours, and uniformly mixing the red mud and the fly ash in a mixer for 3 hours, wherein the adding amount of the red mud is 49.75 wt%, the adding amount of the fly ash is 49.75 wt%, and the adding amount of a foaming agent is 0.5 wt%;
pressing to form a blank and processing: keeping the pressure of the uniformly mixed pre-foaming powder raw materials at 300MPa for 120s to press the uniformly mixed pre-foaming powder raw materials into a cylindrical blank with the diameter of 20 multiplied by 5mm, and drying the demolded blank in a drying oven at the temperature of 100 ℃ for 12 h;
foaming procedure and temperature reduction: and putting the dried sample into a mullite box, heating to 1280 ℃ in a high-temperature furnace, and keeping the temperature for 90min to obtain the novel red mud-fly ash porous ceramic, wherein the holes are distributed in the vertical section direction to form a gradient structure.
The foregoing is merely a preferred embodiment of the invention, which is intended to be illustrative and not limiting. It will be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. A method for preparing novel porous ceramic with a gradient structure by utilizing red mud-fly ash is characterized by comprising the following steps:
s1, pretreating red mud and fly ash: crushing red mud blocks, drying and sieving to obtain red mud, wherein the fly ash is first-grade ash;
s2, mixing the powder: mixing the screened red mud, the screened fly ash and a foaming agent to obtain a porous ceramic powder raw material;
s3, pressing into a blank and foaming: and (2) carrying out compression molding on the porous ceramic powder raw material to obtain a high-temperature pre-foamed blank, drying the blank at a drying temperature, carrying out high-temperature foaming and heat preservation to obtain the porous ceramic with uniform plane aperture and gradient structural hole arrangement on a vertical section.
2. The method for preparing a novel porous ceramic with a gradient structure from red mud-fly ash according to claim 1, wherein in step S1, the crushing treatment time of the red mud blocks in a crusher is 1min to 5min, the crushed red mud blocks are dried at 100 ℃ for 12h and then screened, and the granularity of the red mud obtained after complete screening is 100 meshes to 400 meshes.
3. The method for preparing a novel porous ceramic with a gradient structure from red mud-fly ash as claimed in claim 1, wherein in step S2, 50-90% by mass of the red mud and 10-50% by mass of the fly ash are mixed, and the addition amount of the foaming agent is 0.5-1.5 wt%.
4. The method for preparing the novel gradient-structure porous ceramic by using the red mud-fly ash as claimed in claim 3, wherein the foaming agent is one or a mixture of more of silicon carbide, calcium carbonate, fluorite, calcium sulfate and manganese dioxide.
5. The method for preparing a novel porous ceramic with a gradient structure from red mud-fly ash according to claim 1, wherein in step S2, the mixing time of the red mud, the fly ash and the foaming agent in a mixer is 1-3 h.
6. The method for preparing a novel porous ceramic with a gradient structure from red mud-fly ash according to claim 1, wherein in step S3, the pressure for pressing the porous ceramic powder raw material is 50 MPa-300 MPa, the drying temperature of the green body is 100 ℃ to 140 ℃, and the drying time is 6 h-12 h.
7. The method for preparing a novel porous ceramic with a gradient structure from red mud-fly ash according to claim 6, wherein the temperature in the high-temperature foaming process in the step S3 is controlled as follows: when the current temperature is lower than 300 ℃, the heating rate is 4-8 ℃/min; keeping the temperature for 20-60 min when the current temperature is 300 ℃; when the current temperature is higher than 300 ℃, the heating rate is 3 ℃/min-5 ℃/min until the foaming temperature is reached, and the temperature is kept, wherein the foaming temperature is 1220-1280 ℃, and the temperature is kept for 30 min-90 min.
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