CN112028662A - Composite hierarchical pore structure ceramic and preparation method thereof - Google Patents
Composite hierarchical pore structure ceramic and preparation method thereof Download PDFInfo
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- CN112028662A CN112028662A CN202010736797.7A CN202010736797A CN112028662A CN 112028662 A CN112028662 A CN 112028662A CN 202010736797 A CN202010736797 A CN 202010736797A CN 112028662 A CN112028662 A CN 112028662A
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/138—Waste materials; Refuse; Residues from metallurgical processes, e.g. slag, furnace dust, galvanic waste
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
The invention discloses a composite hierarchical porous structure ceramic and a preparation method thereof, wherein the composite hierarchical porous structure ceramic comprises steel slag, kieserite, a polyoxyethylene polyoxypropylene ether segmented copolymer solution, a mesoporous template agent, an isobutylene-maleic anhydride copolymer and water; the preparation method comprises mixing steel slag, brucite, polyoxyethylene polyoxypropylene ether block copolymer solution, mesoporous template agent and isobutylene-maleic anhydride copolymer, mixing with water to obtain slurry, injecting the slurry into a mold for gel reaction to obtain a blank, drying, calcining, and cooling. The ceramic has a fine and uniform mesoporous structure on the wall of the original macroporous structure, namely a macro-pore structure of 50-200 mu m and a mesoporous structure of 20-50 nm, wherein the macro-pore structure has both open pores and closed pores and has ultrahigh porosity and specific surface area; in addition, the preparation process of the ceramic is simple and the cost is low.
Description
Technical Field
The invention belongs to the field of ceramic preparation, and particularly relates to composite hierarchical pore structure ceramic and a preparation method thereof.
Background
The porous ceramic has the characteristics of low density, light weight, high porosity, small heat conductivity coefficient and the like. Porous materials can be divided into three types based on the size of the pore diameter: macroporous materials with the aperture larger than 50nm, mesoporous materials with the aperture between 2nm and 50nm and mesoporous materials with the aperture smaller than 2 nm.
With the rapid development of modern industry, the requirement on the comprehensive performance of the porous ceramic material is higher and higher, the performance of the porous ceramic with single pore diameter has certain limitation, and the multi-level pore material has the advantages of good permeability, developed pore structure, large specific surface area and pore volume and the like, and breaks through the limitation of single pore structure of the traditional single-level pore material.
However, how to simply, efficiently and inexpensively construct the porous ceramics with the hierarchical pore structure is a problem to be solved at present.
Disclosure of Invention
The purpose of the invention is as follows: the first object of the present invention is to provide a ceramic having a hierarchical pore structure having both a macroporous structure and a mesoporous structure;
the second purpose of the invention is to provide a preparation method of the ceramic.
The technical scheme is as follows: the ceramic with the macroporous-mesoporous composite hierarchical pore structure comprises the following raw materials in percentage by mass: 35-40% of steel slag, 10-15% of kieserite, 0.5-1% of polyoxyethylene polyoxypropylene ether block copolymer, 1.5-2% of mesoporous template agent, 7-8% of isobutene-maleic anhydride copolymer and 40-45% of water.
According to the invention, steel slag, kieserite, a polyoxyethylene polyoxypropylene ether block copolymer, a mesoporous template and an isobutylene-maleic anhydride copolymer are compounded, so that the prepared ceramic has a macro-pore structure of 50-200 mu m and a mesoporous structure of 20-50 nm, and the macro-pore structure has both open pores and closed pores; wherein, the raw materials mainly comprise metallurgical steel slag and kieserite, the fired porous ceramic crystalline phase comprises magnesian rosepside and gehlenite, and the mechanical strength is higher; the multi-stage composite pore structure is prepared by combining the method of preparing macropores by directly foaming the polyoxyethylene polyoxypropylene ether block copolymer and preparing a mesoporous structure by adopting a mesoporous template agent, the porous ceramic with the multi-stage composite pore structure has a fine and uniform mesoporous structure on the pore wall of the original macroporous structure, and meanwhile, the addition of the polyoxyethylene polyoxypropylene ether block copolymer can reduce the mesoporous order degree of the mesoporous template agent, is more beneficial to forming irregular pores and further reduces the density of the porous ceramic. In addition, under the effect of co-pore formation of the polyoxyethylene polyoxypropylene ether block copolymer and the mesoporous template, the density of the porous ceramic is favorably further reduced, so that the porous ceramic with ultrahigh porosity and specific surface area is prepared.
Preferably, the steel slag used in the invention has a particle size of 0.4-200 μm. The particle size of the kieserite can be 0.4-200 mu m. The steel slag and the kieserite with the grain diameter of 0.4-200 mu m are adopted, so that more uniform porous ceramic slurry can be prepared, the specific surface area of the ceramic raw material and the contact area among the components can be increased, the growth and development of the crystal grains of the gehlenite-magadite complex phase ceramic in the sintering process are promoted, and the mechanical strength of the porous ceramic is improved.
Furthermore, the mass fraction of the polyoxyethylene polyoxypropylene ether segmented copolymer solution adopted by the invention is 14-20%. The mesoporous template can be polyethylene glycol, tert-butyl alcohol, oligopeptide or polyamide.
The method for preparing the ceramic comprises the following steps: uniformly mixing steel slag, kieserite, a polyoxyethylene polyoxypropylene ether segmented copolymer solution, a mesoporous template agent and an isobutylene-maleic anhydride copolymer according to mass fraction, fully mixing with water to prepare slurry, injecting the slurry into a mold to carry out gel reaction to prepare a blank body, and drying, calcining and cooling to prepare the ceramic.
Furthermore, when the ceramic is prepared, the gel reaction is carried out for 4-6 hours at room temperature under the air atmosphere. The drying is carried out for 12-24 h at 50-60 ℃. The calcination is carried out by raising the temperature to 850-950 ℃ at a heating rate of 1-2 ℃/min, keeping the temperature for 2-3 h, raising the temperature to 1150-1200 ℃ at a heating rate of 3-8 ℃/min, and keeping the temperature for 30-60 min.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: the ceramic has a fine and uniform mesoporous structure on the wall of the original macroporous structure, namely a macro-pore structure of 50-200 mu m and a mesoporous structure of 20-50 nm, wherein the macro-pore structure has both open pores and closed pores, and has ultrahigh porosity and specific surface area, and the density is less than 250kg/m3The compressive strength reaches 1.4MPa, and the flexural strength reaches 0.6 MPa; in addition, the preparation process of the ceramic is simple, the cost is low, expensive production equipment is not needed, and the ceramic has potential application value.
Drawings
FIG. 1 is an SEM image of the macroporous structure of the porous ceramic of the present invention;
FIG. 2 is a SEM image of the mesoporous structure of the porous ceramic of the present invention;
FIG. 3 is an X-ray diffraction pattern of the porous ceramic of the present invention.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to the following examples. The raw materials adopted by the invention are the conventional and well-known raw materials, and can be purchased from the market. The solvent of the polyoxyethylene polyoxypropylene ether block copolymer solution is deionized water.
Example 1
The porous ceramics of this example used the raw materials shown in table 1 below.
Table 1 porous ceramic raw material of example 1
Raw materials | Components |
Steel slag | 35 |
|
10 |
Polyoxyethylene polyoxypropylene ether block copolymer solution | 0.5 |
Tert-butyl alcohol | 1.5 |
Isobutylene-maleic anhydride copolymer | 8 |
Water (W) | 45 |
The preparation method of the porous ceramic comprises the following steps:
(1) fully and uniformly mixing steel slag, kieserite, polyoxyethylene polyoxypropylene ether segmented copolymer, tertiary butanol, isobutylene-maleic anhydride copolymer and water to prepare mixed slurry;
(2) injecting the mixed slurry into a 40 x 160mm mold, and carrying out gel reaction on the mold and the slurry for 4-6 h under the conditions of room temperature and air atmosphere to obtain a blank;
(3) and (3) demolding the blank, placing the blank in a drying oven at 50 ℃ for drying for 12h, then raising the temperature to 850 ℃ at the heating rate of 1-2 ℃/min, preserving the heat for 2h, then raising the temperature to 1150-1200 ℃ at the heating rate of 3-8 ℃/min, preserving the heat for 30min, and naturally cooling to room temperature to obtain the ceramic.
Example 2
The porous ceramics of this example used the raw materials shown in table 2 below.
Table 2 porous ceramic raw material of example 2
The porous ceramic was prepared in the same manner as in example 1.
Example 3
The porous ceramics of this example used the raw materials shown in table 3 below.
Table 3 porous ceramic feedstock of example 3
Raw materials | Components |
Steel slag | 35 |
Brucite | 15 |
Polyoxyethylene polyoxypropylene |
1 |
Polyamide | 2 |
Isobutylene-maleic anhydride copolymer | 7 |
Water (W) | 40 |
The porous ceramic was prepared in the same manner as in example 1.
Example 4
The porous ceramics of this example used the raw materials shown in table 4 below.
Table 4 porous ceramic feedstock of example 4
Raw materials | |
Steel slag | |
40 | |
|
10 |
Polyoxyethylene polyoxypropylene |
1 |
Oligopeptide | 2 |
Isobutylene-maleic anhydride copolymer | 7 |
Water (W) | 40 |
The porous ceramic was prepared in the same manner as in example 1.
Performance detection
The density of the ceramics prepared in the above examples was obtained by mass to volume ratio, and the compressive strength was tested using a full automatic compression bender (WHY-200). The results obtained are shown in table 5 below.
TABLE 5 porous ceramic Properties
As can be seen from Table 5, the porous Mg-rosmarinum-gehlenite composite ceramic prepared by the invention has smaller density change amplitude, wherein the density of example 4 is reduced to 186kg/m3And the density is lower. The compressive strength and the flexural strength of examples 1 to 4 were all 1.4MPa or more and 0.6MPa or more, respectively.
In addition, the ceramics prepared in example 1 were subjected to electron microscopy and XRD examination, and the results obtained are shown in fig. 1 to 3. As can be seen from the graphs in FIGS. 1 and 2, the size of the macro pores of the porous ceramic prepared by the method is 50-200 μm, the mesoporous structure on the walls of the macro pores is 20-50 nm, the mesoporous order degree is low, and the pores are distributed irregularly, so that the method for preparing the multi-stage composite pore structure by combining the polyoxyethylene polyoxypropylene ether block copolymer and the mesoporous template agent is verified, the mesoporous order degree is reduced, and the density of the porous ceramic is reduced. As can be seen from the graph 3, when the ceramic is prepared, after sintering at 1150-1200 ℃, the porous ceramic has a magnesian rosepside phase and a gehlenite phase, the phase structure is complete, and the magnesian rosepside-gehlenite complex-phase ceramic is generated after sintering at 1150-1200 ℃.
Besides the above embodiments, the ceramic can be dried and reacted at 60 ℃ for 24 hours, and the ceramic can be calcined at a temperature rise rate of 1-2 ℃/min to 950 ℃ and then at a temperature rise rate of 3-8 ℃/min to 1200 ℃ after heat preservation for 3 hours, and the effect difference is small.
Claims (9)
1. The composite hierarchical pore structure ceramic is characterized by comprising the following raw materials in percentage by mass: 35-40% of steel slag, 10-15% of kieserite, 0.5-1% of polyoxyethylene polyoxypropylene ether block copolymer solution, 1.5-2% of mesoporous template agent, 7-8% of isobutylene-maleic anhydride copolymer and 40-45% of water.
2. The composite hierarchical pore structural ceramic of claim 1, wherein: the particle size of the steel slag is 0.4-200 mu m.
3. The composite hierarchical pore structural ceramic of claim 1, wherein: the particle size of the kieserite is 0.4-200 mu m.
4. The composite hierarchical pore structural ceramic of claim 1, wherein: the mass fraction of the polyoxyethylene polyoxypropylene ether segmented copolymer solution is 12-20%.
5. The composite hierarchical pore structural ceramic of claim 1, wherein: the mesoporous template is polyethylene glycol, tert-butyl alcohol, oligopeptide or polyamide.
6. A method of making the ceramic of claim 1, comprising the steps of: uniformly mixing steel slag, kieserite, a polyoxyethylene polyoxypropylene ether segmented copolymer solution, a mesoporous template agent and an isobutylene-maleic anhydride copolymer according to mass fraction, fully mixing with water to prepare slurry, injecting the slurry into a mold to carry out gel reaction to prepare a blank body, and drying, calcining and cooling to prepare the ceramic.
7. The method of claim 6, wherein: the gel reaction is carried out for 4-6 h at room temperature under the air atmosphere.
8. The method of claim 6, wherein: the drying is carried out for 12-24 h under the condition of 50-60 ℃.
9. The method of claim 6, wherein: the calcination is carried out by raising the temperature to 850-950 ℃ at a heating rate of 1-2 ℃/min, keeping the temperature for 2-3 h, raising the temperature to 1150-1200 ℃ at a heating rate of 3-8 ℃/min, and keeping the temperature for 30-60 min.
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CN114988851A (en) * | 2022-07-14 | 2022-09-02 | 山东理工大学 | Method for preparing lightweight porous ceramic material by efficiently utilizing steel slag |
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