CN112851314A - Method for preparing porous ceramic based on particle size and reaction activity control and porous ceramic - Google Patents

Method for preparing porous ceramic based on particle size and reaction activity control and porous ceramic Download PDF

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CN112851314A
CN112851314A CN202110134252.3A CN202110134252A CN112851314A CN 112851314 A CN112851314 A CN 112851314A CN 202110134252 A CN202110134252 A CN 202110134252A CN 112851314 A CN112851314 A CN 112851314A
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porous ceramic
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CN112851314B (en
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陈松
蒋小松
孙红亮
王良辉
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Southwest Jiaotong University
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Abstract

The invention discloses a method for preparing porous ceramic based on particle size and reaction activity control and the porous ceramic, wherein the porous ceramic comprises the following chemical structure expression: xB2O3·ySiO2·uAl2O3·vN2O. wZO, wherein N is2O is Na2O or K2O and ZO are MgO, CaO, SrO, BaO or ZnO, x, y, u, v and w are molar ratios, x is more than or equal to 0.5 and less than or equal to 2, y is more than or equal to 1 and less than or equal to 4, u is more than or equal to 0.1 and less than or equal to 1, v is more than or equal to 0.01 and less than or equal to 0.1, and w is more than or equal to 0.01 and less than or equal to 0.1. The preparation method comprises the following steps: s1, weighing the raw materials according to the raw material composition, adding water, and ball-milling for 1-3h to obtain a mixture; s2, separating out ceramic suspension slurry in the mixture obtained in the S1, drying to constant weight to obtain a dry sample, and then crushing and grinding the dry sample to obtain a powdery material; s3, performing powder granulation and molding on the powdery material obtained in the step S2, and sintering at the temperature of 800-950 ℃ for 2-3h to obtain the material. The invention is prepared by the formulaControlling and multi-ion doping to adjust the reaction activity to control the generated pores, and regulating and controlling the porosity of the quartz glass powder under the control of the particle size of the quartz glass powder.

Description

Method for preparing porous ceramic based on particle size and reaction activity control and porous ceramic
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a method for preparing porous ceramic based on particle size and reaction activity control and the porous ceramic.
Background
The porous ceramic material is prepared from certain raw materials and additives through a forming and sintering process, has a certain porosity, and has the characteristics of temperature resistance, high pressure resistance, acid, alkali and organic medium corrosion resistance, good biological inertia, controllable pore structure, corresponding porosity and the like according to application requirements. According to the industrial requirements, the catalyst can be applied to filtration and separation of media, environmental protection and sound insulation, gas distribution, catalyst carriers, diaphragms and the like. In general, porous ceramics can be classified into foamed ceramics, honeycomb ceramics and granular ceramics, and their porosities are generally 89 to 90%, 70%, 30 to 50%, respectively. The main preparation methods for producing the appropriate porosity include an additive pore-forming agent method, a foaming method, an organic foam impregnation method and a sol-gel method. Because of the defects of poor reproducibility, high cost, difficult control of the pore structure and the like, the application of the porous material is restricted, and the application performance of the porous material still needs to be improved by perfecting the preparation process, improving the material quality, coordinating the relationship between the porosity and the strength and the like.
Disclosure of Invention
The invention aims to: aiming at the defects in the prior art, the method for preparing the porous ceramic based on particle size and reaction activity control and the porous ceramic are provided.
The technical scheme adopted by the invention is as follows:
a porous ceramic prepared based on particle size and reactivity control comprises the following chemical structure expression:
xB2O3·ySiO2·uAl2O3·vN2o. wZO, wherein N is2O is Na2O or K2O and ZO are MgO, CaO, SrO, BaO or ZnO, x, y, u, v and w are molar ratios, x is more than or equal to 0.5 and less than or equal to 2, y is more than or equal to 1 and less than or equal to 4, u is more than or equal to 0.1 and less than or equal to 1, v is more than or equal to 0.01 and less than or equal to 0.1, and w is more than or equal to 0.01 and less than or equal to 0.1.
Further, the chemical structure expression is included as follows:
xB2O3·ySiO2·uAl2O3·vK2o wBaO or xB2O3·ySiO2·uAl2O3·vNa2O.wCaO or xB2O3·ySiO2·uAl2O3·vK2O.wSrO, wherein x is more than or equal to 0.5 and less than or equal to 2, y is more than or equal to 1 and less than or equal to 4, u is more than or equal to 0.1 and less than or equal to 1, v is more than or equal to 0.05 and less than or equal to 0.1, and w is more than or equal to 0.01 and less than or equal to 0.1.
Further, the specific chemical structure expression is as follows:
0.9B2O3·2.3SiO2·0.23Al2O3·0.08K2o0.02 BaO or 1.5B2O3·3SiO2·0.3Al2O3·0.01Na2O0.05 CaO or B2O3·2.1SiO2·0.15Al2O3·0.02K2O·0.07SrO。
A raw material for preparing the above porous ceramic prepared based on particle size and reactivity control, comprising at least one of the following components:
60-200 mesh quartz glass powder and H3BO3、NaOH、KOH、Ba(OH)2·8H2O、Al(OH)3、MgO、Ca(OH)2、Sr(OH)2·8H2O、Mg(OH)2And ZnO.
The method for preparing the porous ceramic by adopting the raw materials based on particle size and reaction activity control comprises the following steps:
s1, weighing the raw materials according to the raw material composition, adding water, and ball-milling for 1-3h to obtain slurry;
s2, drying the slurry obtained in the step S1 to constant weight to obtain a dry sample, and then crushing and grinding the dry sample to obtain a powdery material;
s3, performing powder granulation and molding on the powdery material obtained in the step S2, and sintering at the temperature of 800-950 ℃ for 2-3h to obtain the material.
The principle of the invention is as follows: according to the invention, the quartz glass powder with multiple particle sizes and boric acid are used as main raw materials, and the quartz glass powder with multiple particle sizes and the boric acid have higher reaction activity during sintering, so that pores are generated in a final ceramic structure due to the occurrence and slight overburning of a large amount of borosilicate glass phase, and a certain porosity is formed due to the addition of the quartz glass aggregate with large particle size and the bonding effect of glass.
To improve the bonding ability of glass and effectively control the reactivity so as not to cause voidsRate runaway, composition by addition of Al (OH)3And other alkali metal and alkaline earth metal compounds, specifically by Al (OH)3And the amount of alkali metal or alkaline earth metal ions added is controlled and the porosity of the borosilicate is controlled by suppressing the overburning reaction of the borosilicate based on the chemical bonding between the added ions and the network ions. Meanwhile, as the 60-200-mesh quartz glass powder is adopted, the porosity is physically controlled in an auxiliary manner through the mixing ratio of the quartz glass powder with different particle sizes, and a porous structure with the porosity between 17-35% is realized.
Further, the liquid-solid ratio of the mixture in the S1 is 3-5: 1; preferably 4: 1.
Further, drying the mixture in S2 for 24-36h at 70-90 ℃.
Further, drying at 80 ℃ for 30h in S2.
Further, the particle size of the powdery material obtained in S2 is 30 to 150. mu.m.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the invention, pores are generated through the reaction activity of boric acid and quartz glass powder in the self components, and the preparation method of the porous ceramic with adjustable pores is realized under the regulation and control of the doping of the aggregate and the compound, so that the production of the porous ceramic by complex processes such as a foaming agent is avoided, the dependence on the foaming agent and a pore-forming agent in the production process of the porous ceramic is reduced, the process is simplified, and the cost is reduced;
2. boric acid and quartz glass powder are used as main raw materials, the reaction activity is adjusted and controlled to generate pores through regulation and control of a formula and multi-ion doping, the porosity of the quartz glass powder is regulated and controlled under the control of the particle size of the quartz glass powder, and porous ceramic with adjustable porosity is prepared at a lower sintering temperature;
3. the porous ceramic prepared by the invention has uniform pores, the porosity is between 17 and 35 percent, the pores are adjustable, the bending strength is high and is more than 20MPa, and the porous ceramic has better physical properties.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a structural representation diagram of embodiment 1 of the present invention;
FIG. 2 is a structural representation diagram of embodiment 2 of the present invention;
FIG. 3 is a structural representation diagram of embodiment 3 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The preferred embodiment of the invention provides a method for preparing porous ceramic based on particle size and reaction activity control, which comprises the following specific steps:
(1) taking solid raw materials of boric acid, quartz glass powder, potassium hydroxide and barium hydroxide octahydrate according to the molar ratio of chemical elements of 0.9B2O3·2.3SiO2·0.23Al2O3·0.08K2The composition of O.0.02 BaO is proportionally weighed and then put into a ball milling tank; wherein the quartz glass powder with the grain diameter of 100 meshes accounts for 40 percent, and the quartz glass powder with the grain diameter of 200 meshes accounts for 60 percent;
(2) adding deionized water for ball milling, using water as a ball milling medium, and mixing the deionized water and the solid raw materials according to a liquid-solid ratio of 4:1, adding distilled water to prepare a mixture; ball milling time is 2 hours;
(3) after the ball milling is finished, pouring out the slurry and drying the slurry for 24 hours at the temperature of 80 ℃;
(4) after drying, powder granulation, molding and sintering are carried out, the sintering temperature is set at 900 ℃, the sintering time is 2 hours, a sample is obtained, the sample is marked as embodiment 1, and the characteristic structure is shown in figure 1.
Example 2
The preferred embodiment of the invention provides a method for preparing porous ceramic based on particle size and reaction activity control, which comprises the following specific steps:
(1) taking solid raw materials of boric acid, quartz glass powder, sodium hydroxide and calcium hydroxide according to the molar ratio of chemical elements of 1.5B2O3·3SiO2·0.3Al2O3·0.01Na2O.0.05 CaO, and putting the mixture into a ball milling tank after proportioning and weighing; wherein the quartz glassIn the powder, quartz glass powder with the grain diameter of 60 meshes accounts for 80 percent, and quartz glass powder with the grain diameter of 100 meshes accounts for 20 percent;
(2) adding deionized water for ball milling, using water as a ball milling medium, and mixing the deionized water and the solid raw materials according to a liquid-solid ratio of 4:1, adding distilled water to prepare a mixture; ball milling time is 2 hours;
(3) after the ball milling is finished, pouring out the slurry and drying the slurry for 29 hours at the temperature of 80 ℃;
(4) after drying, powder granulation, molding and sintering are carried out, the sintering temperature is set at 950 ℃, the sintering time is 2 hours, a sample is obtained, the sample is marked as embodiment 2, and the characteristic structure is shown in figure 2.
Example 3
The preferred embodiment of the invention provides a method for preparing porous ceramic based on particle size and reaction activity control, which comprises the following specific steps:
(1) taking solid raw materials of boric acid, 100-mesh quartz glass powder, potassium hydroxide and strontium carbonate according to the molar ratio of chemical elements B2O3·2.1SiO2·0.15Al2O3·0.02K2The composition of O.0.07 SrO is proportionally weighed and then is put into a ball milling tank;
(2) adding deionized water for ball milling, using water as a ball milling medium, and mixing the deionized water and the solid raw materials according to a liquid-solid ratio of 4:1, adding distilled water to prepare a mixture; ball milling time is 2.5 hours;
(3) after the ball milling is finished, pouring out the slurry and drying the slurry for 23 hours at the temperature of 90 ℃;
(4) after drying, powder granulation, molding and sintering are carried out, the sintering temperature is set at 850 ℃, the sintering time is 2 hours, a sample is obtained, the sample is marked as embodiment 3, and the characteristic structure is shown in figure 3.
Examples of the experiments
The porosity is tested by mercury pressing method, and the pore diameter and pore distribution of coke are determined by applying external pressure to make mercury enter coke pores by overcoming surface tension. The additional pressure is increased to allow mercury to enter the smaller pores and the more mercury enters the coke pores. The pore volume of the corresponding pore size can be known by measuring the amount of mercury entering the pores under different external pressures. The test was carried out using a mercury intrusion gauge. The porosity of embodiment 1 is 17%, the porosity of embodiment 2 is 30%, and the porosity of embodiment 3 is 34%.
The bending strength is tested by adopting a three-point bending method, and the method refers to the GB/T4741 ceramic material bending strength test method. The flexural strength of embodiment 1 was 45MPa, the flexural strength of embodiment 2 was 35MPa, and the flexural strength of embodiment 3 was 21 MPa.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (8)

1. The porous ceramic prepared based on particle size and reactivity control is characterized by comprising the following chemical structure expression:
xB2O3·ySiO2·uAl2O3·vN2o. wZO, wherein N is2O is Na2O or K2O and ZO are MgO, CaO, SrO, BaO or ZnO, x, y, u, v and w are molar ratios, x is more than or equal to 0.5 and less than or equal to 2, y is more than or equal to 1 and less than or equal to 4, u is more than or equal to 0.1 and less than or equal to 1, v is more than or equal to 0.01 and less than or equal to 0.1, and w is more than or equal to 0.01 and less than or equal to 0.1.
2. The porous ceramic prepared based on particle size and reactivity control according to claim 1, comprising a chemical structure expression as follows:
xB2O3·ySiO2·uAl2O3·vK2o wBaO or xB2O3·ySiO2·uAl2O3·vNa2O.wCaO or xB2O3·ySiO2·uAl2O3·vK2O.wSrO, wherein x is more than or equal to 0.5 and less than or equal to 2, y is more than or equal to 1 and less than or equal to 4, u is more than or equal to 0.1 and less than or equal to 1, v is more than or equal to 0.05 and less than or equal to 0.1, and w is more than or equal to 0.01 and less than or equal to 0.1.
3. The porous ceramic prepared based on particle size and reactivity control according to claim 1, wherein the specific chemical structural expression is as follows:
0.9B2O3·2.3SiO2·0.23Al2O3·0.08K2o0.02 BaO or 1.5B2O3·3SiO2·0.3Al2O3·0.01Na2O0.05 CaO or B2O3·2.1SiO2·0.15Al2O3·0.02K2O·0.07SrO。
4. A raw material for preparing the porous ceramic prepared based on the particle size and reactivity control according to any one of claims 1 to 3, characterized by comprising at least one of the following components:
60-200 mesh quartz glass powder and H3BO3、NaOH、KOH、Ba(OH)2·8H2O、Al(OH)3、MgO、Ca(OH)2、Sr(OH)2·8H2O、Mg(OH)2And ZnO.
5. The method for preparing porous ceramics by using the raw material of claim 4 based on particle size and reactivity control, characterized by comprising the steps of:
s1, weighing the raw materials according to the raw material composition, adding water, and ball-milling for 1-3h to obtain slurry;
s2, drying the slurry obtained in the step S1 to constant weight to obtain a dry sample, and then crushing and grinding the dry sample to obtain a powdery material;
s3, performing powder granulation and molding on the powdery material obtained in the step S2, and sintering at the temperature of 800-950 ℃ for 2-3h to obtain the material.
6. The method as claimed in claim 5, wherein the liquid-solid ratio of the mixture in S1 is 3-5: 1.
7. The method according to claim 5, wherein the drying in S2 is carried out at 70-90 ℃ for 24-36 h.
8. The method as claimed in claim 5, wherein the grain size of the powdery material obtained in S2 is 30-150 μm.
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