CN102718494A - Preparation method of composite silicon carbide ceramic filter membrane material - Google Patents
Preparation method of composite silicon carbide ceramic filter membrane material Download PDFInfo
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Abstract
The invention belongs to the technical field of porous ceramic filter membrane, and relates to a preparation method of composite silicon carbide ceramic filter membrane material. The preparation method includes: well mixing silicon carbide, ceramic binder, pore-forming agent, and cellulose sodium carboxymethyl solution, forming by dry pressing to obtain a green body of a silicon carbide porous ceramic support, spreading and coating a layer of filler powder on surface of the green body, forming by dry pressing, coating ceramic fiber mixture on the surface, forming by dry pressing, coating filter membrane mixture, forming by dry pressing, and sintering to obtain the composite silicon carbide ceramic filter membrane material. The preparation method has the advantages that process is simple, volatile filler is sintered to seal pores on the surface of the support, a ceramic fiber transition layer is introduced, entering of the filter membrane material into base material can be effectively avoided, evener and smoother composite silicon carbide ceramic filter membrane material can be prepared by single sintering, and the preparation method is high in efficiency, low in energy consumption and the like.
Description
Technical field
The invention belongs to ceramic foam filter membrane material technical field, particularly a kind of method that adopts dry-pressing formed and synchronous sintering process to prepare the composite silicon carbide ceramic filter membrane material is mainly used in high-temperature dust removal gas.
Background technology
The utilization of the energy mainly is to obtain through direct burning.Because it is insufficient that the restriction of prior art causes burning, not only efficiency of energy utilization is lower, also gives off a large amount of dust, and environmental pollution is serious.Improve efficiency of energy utilization, reducing dust discharge is the research direction of present materialogy.Ceramic filter tube is widely used in the gas cleaning at high temperature purification techniques, has become the key part that industries such as material, metallurgy, chemical industry, electric power realize gas solid separation, energy-conserving and environment-protective.General two-part structure, i.e. supporter part and the filtering membrane part of adopting of traditional high-strength high temperature-resistant ceramic filter tube.Supporter adopts big particle diameter ceramic particle to prepare, and can mechanical strength be provided for the strainer tube internal layer; The ceramic particle of forming filtering membrane is then less, has guaranteed that whole filtering bodies has enough dust removal by filtration efficient and precision.Traditional ceramic filter tube material; Because the ceramic particle particle diameter of preparation supporter is big, the aperture is big, much larger than the grain diameter of surface film, when making film in its surface; Get into because of the surface film powder in the space of supporter; Thereby increased the filtration pressure drop degree of strainer tube material, increased the thickness of film, influenced the overall performance of strainer tube material.
The composite silicon carbide ceramic filter membrane material is between silicon carbide film and silicon carbide ceramics supporter, to increase the ceramic fiber transition layer, reaches the structure and the performance of improved chimney filter material; This layer of fibers has not only stoped the surface film powder to get into the supporter space, and effectively reduces the filtration pressure drop degree of filtering material.
The ceramic foam filtering membrane is generally through the preparation of slurry coating method, like crystal pulling method, spraying method and doctor-blade casting process etc., still because the hole of ceramic foam base material is more; The aperture is bigger; The surface is unfairness also, directly on ceramic foam base material surface, during coating, three defectives mainly occur: one, because the aperture of base material is bigger; Cause the filtering membrane slurry can get in the base material air, influence its filter effect; Two, because the more and surface irregularity of base material, can not provide the surface of smooth all when being beneficial to coating, the membrane structure that causes coating is rough smooth.Three, the ceramic foam filtering membrane generally is earlier carrying out sintering after the compression moulding of ceramic foam base material, coating on base material then, sintering more at last; Its complicated process of preparation, and length consuming time, power consumption are big.
Summary of the invention
The preparation method who the objective of the invention is to be directed against the deficiency of prior art and a kind of composite silicon carbide ceramic filter membrane material is provided; Adopt dry-pressing formed and synchronous sintering process; On the porous ceramic support surface, be coated with earlier the volatilizable spackling of shop compacting one deck sintering; Press ceramic layer of fibers in its surface again, rete is filtered in compacting on fiber layer surface at last.Spackling can avoid ceramic fiber to get in the base material effectively with the shutoff of supporting body surface hole; Owing to utilize dry-pressing formedly, make that the surface of each layer is comparatively smooth smooth, for each rete moulding provides smooth slick surface, help preparing more evenly, more smooth complex silicon carbide filter membrane material base substrate; Simultaneously, only need carry out once sinteredly can obtaining the composite silicon carbide ceramic filter membrane material; Have characteristics such as technology is simple, efficient is high, energy consumption is low.
The technical scheme that the present invention adopted:
A kind of preparation method of composite silicon carbide ceramic filter membrane material, its step is following:
1, silit, vitrified bond, pore-forming material and carboxymethyl cellulose being received (CMC) solution, to receive the mass ratio of (CMC) solution by silit, vitrified bond, pore-forming material and carboxymethyl cellulose be that the mixed of 10:0.5～3.3:0.5～4.0:1.0～3.0 back that stirs is dry-pressing formed; Obtain carborundum porous ceramics supporter base substrate; Pressure is 10～100MPa, and wherein to receive the mass concentration of (CMC) solution be 1wt%～4wt% to carboxymethyl cellulose.
Said vitrified bond is that the quartzy mixing and ball milling configuration of 65wt% potassium felspar sand, 12wt% kaolin and 23wt% forms by massfraction.
The grain diameter of said vitrified bond powder is 0.1～3 μ m.
The particle diameter of said silit is 180～350 μ m.
Said pore-forming material is a gac, and its grain diameter is 0.1～5 μ m.
2, on carborundum porous ceramics supporter billet surface, be coated with the volatilizable spackling powder of shop one deck sintering and dry-pressing formed, pressure is 1～5MPa.Being coated with the shop spackling can stop up supporter billet surface space, avoids the film powder to get in the space of supporter.
Said spackling powder diameter is 0.1～5 μ m.
Said spackling is gac or graphite.
3, the equal length of making even is the mullite fiber of 10mm, is that the mixed of 1:0.3～1.5 stirs and obtains the ceramic fiber compound by the mass ratio of mullite fiber, vitrified bond; The ceramic fiber transition layer evenly is coated with is layered on step 2) on the gained section bar surface, and dry-pressing formed, pressure is 1～5 MPa.
Single diameter Distribution 1～15 μ m of said mullite fiber, length-to-diameter ratio is greater than 10.
4, the mass ratio by sic powder, vitrified bond is the mixed of 10:0.5～3.3 and stirs, and obtains the filtering membrane compound, the filtering membrane compound evenly is coated be layered on the step 3) gained section bar surface, and dry-pressing formed, pressure is 1～5 MPa.
In the filtering membrane compound, when, pressure less when the ceramic bonding agent content was big, porosity was bigger, and the filtering membrane after dry-pressing formed can satisfy the respective performances requirement.When vitrified bond more for a long time, porosity is little, need in the filtering membrane compound, add pore-forming material and improve porosity, the massfraction of the pore-forming material that is added is below 30wt%.
5, step 4) gained section bar is carried out sintering, sintering temperature is 1100～1500
oC, temperature rise rate 1～10
oC/min, soaking time is 1～3h, gets the composite silicon carbide ceramic filter membrane material.
Technology of the present invention is simple; Adopt dry-pressing formed and synchronous sintering process; On the silicon carbide ceramics supporting body surface, be coated with of the hole shutoff of compacting one deck sintering volatilizable spackling in shop with supporting body surface; And between silicon carbide film and silicon carbide ceramics supporter, introduce the ceramic fiber transition layer, and avoid filter membrane material to get in the base material effectively, can not only the smooth surface that help moulding be provided for preparing ceramic fiber transition layer and superficial film; And only need once sinteredly can to prepare more evenly, more smooth composite silicon carbide ceramic filter membrane material, have characteristics such as efficient height, energy consumption are low.
Description of drawings
Fig. 1 is the SEM figure on composite silicon carbide ceramic filter membrane material provided by the invention surface.
Fig. 2 is the SEM figure of composite silicon carbide ceramic filter membrane material section provided by the invention.
Embodiment
Below in conjunction with embodiment, specific embodiments of the invention describes in further detail.Following examples are used to explain the present invention, but are not used for limiting scope of the present invention.
Embodiment one
1, be 65wt% potassium felspar sand, 12wt% kaolin, 23wt% quartz by massfraction, getting potassium felspar sand, kaolin and quartzy mixing and ball milling to grain diameter respectively is 0.1～3 μ m, obtains vitrified bond.
2, taking by weighing 10g silicon-carbide particle, 1.11g vitrified bond, 1.33g gac (particle diameter 3 μ m) and 1.5g massfraction respectively is that the carboxymethyl cellulose of 2wt% is received (CMC) solution; At first silicon-carbide particle is added in the CMC solution, and stir; Respectively vitrified bond and gac are added, and after being stirred to evenly, claim its 4g compound and dry-pressing formed, pressure is about 26MPa, obtains carborundum porous ceramics supporter base substrate, diameter 20mm, and thickness is about 5mm.Wherein the median size of silicon-carbide particle is 300 μ m.
3, (particle diameter is 3 μ m to disperse to be coated with shop layer of active carbon powder in the supporter billet surface.), and dry-pressing formed, pressure is about 2MPa.
4, get 1g mullite fiber, the mixing of 0.88g vitrified bond, and stir, promptly make the ceramic fiber compound.Active carbon layer surface upper surface on the supporter billet surface disperses to be coated with shop ceramic fiber compound, and dry-pressing formed, the about 2MPa of pressure.
5,1g sic powder, 0.17g vitrified bond, 0.17g pore-forming material are mixed; And stir; Get filtering membrane compound (wherein the median size of sic powder is 23 μ m, the massfraction 15wt% of vitrified bond, the massfraction 15wt% of pore-forming material gac).On the ceramic fiber laminar surface on the supporter billet surface, disperse to be coated with shop filtering membrane compound, and dry-pressing formed, pressure is about 1.5MPa.
6, step 5) gained section bar is carried out sintering, sintering temperature 1300
oC, temperature rise rate 5
oC, soaking time is 2h, can make the composite silicon carbide ceramic filter membrane material.
Assay: the surperficial SEM Photomicrograph of gained composite silicon carbide ceramic filter membrane material is as shown in Figure 1, and the composite silicon carbide ceramic filter membrane surface is smooth, the even aperture distribution defective is few; The mean porosities 46% of surface filtration film, mean pore size 10 μ m.Its section SEM Photomicrograph is as shown in Figure 2, and composite silicon carbide ceramic filters thickness and is evenly distributed, and does not see that the ceramic fiber transition layer gets into supporter and stops up the duct, and the ceramic fiber transition layer has played to build bridge and accepted effect simultaneously.
Embodiment two
1, with the step (1) of embodiment one.
2, taking by weighing 10g silicon-carbide particle, 1.85g vitrified bond, 2.13g gac (particle diameter 4 μ m) and 1.9g massfraction respectively is that the carboxymethyl cellulose of 3wt% is received (CMC) solution; At first silicon-carbide particle is added in the CMC solution, and stir; Respectively vitrified bond and gac are added, and after being stirred to evenly, claim its 4g compound and dry-pressing formed, pressure is about 26MPa, obtains carborundum porous ceramics supporter base substrate, diameter 20mm, and thickness is about 5mm.Wherein the median size of silicon-carbide particle is 250 μ m.
3, (particle diameter is 0.7 μ m to disperse to be coated with shop one deck powdered graphite in the supporter billet surface.), and dry-pressing formed, pressure is about 4MPa.
4, get 1g mullite fiber, the mixing of 0.5g vitrified bond, and stir, promptly make the ceramic fiber compound.Active carbon layer surface upper surface on the supporter billet surface disperses to be coated with shop ceramic fiber compound, and dry-pressing formed, the about 2MPa of pressure.
5,1g sic powder, 0.24g vitrified bond, 0.32g pore-forming material are mixed, and stir, get the filtering membrane compound.On the ceramic fiber laminar surface on the supporter billet surface, disperse to be coated with shop filtering membrane compound, and dry-pressing formed, pressure is about 2.5MPa.
6, step 5) gained section bar is carried out sintering, sintering temperature 1200
oC, 8 ℃ of temperature rise rates, soaking time is 1h, can make the composite silicon carbide ceramic filter membrane material.
Embodiment three
1, with the step (1) of embodiment one.
2, taking by weighing 10g silicon-carbide particle, 2.68g vitrified bond, 3.45g gac (particle diameter 3 μ m) and 2.5g massfraction respectively is that the carboxymethyl cellulose of 2wt% is received (CMC) solution; At first silicon-carbide particle is added in the CMC solution, and stir; Respectively vitrified bond and gac are added, and after being stirred to evenly, claim its 4g compound and dry-pressing formed, pressure is about 26MPa, obtains carborundum porous ceramics supporter base substrate, diameter 20mm, and thickness is about 5mm.Wherein the median size of silicon-carbide particle is 220 μ m.
3, (particle diameter is 3 μ m to disperse to be coated with shop layer of active carbon powder in the supporter billet surface.), and dry-pressing formed, pressure is about 3MPa.
4, get 1g mullite fiber, the mixing of 1.2g vitrified bond, and stir, promptly make the ceramic fiber compound.Active carbon layer surface upper surface on the supporter billet surface disperses to be coated with shop ceramic fiber compound, and dry-pressing formed, the about 3MPa of pressure.
5,1g sic powder, 0.054g vitrified bond are mixed, and stir, get the filtering membrane compound.On the ceramic fiber laminar surface on the supporter billet surface, disperse to be coated with shop filtering membrane compound, and dry-pressing formed, pressure is about 3.5MPa.
6, step 5) gained section bar is carried out sintering, sintering temperature 1400
oC, 8 ℃ of temperature rise rates, soaking time is 2h, can make the composite silicon carbide ceramic filter membrane material.
Assay: the surfacing of gained composite silicon carbide ceramic filter membrane material, even aperture distribution defective are few; The mean porosities 44% of surface filtration film, mean pore size 12 μ m; Composite silicon carbide ceramic filters thickness and is evenly distributed, and does not see that the ceramic fiber transition layer gets into supporter and stops up the duct, and the ceramic fiber transition layer has played to build bridge and accepted effect simultaneously; It is not tight that but supporter, ceramic fiber transition layer and surface carborundum film three are connected, and the upper layer filtering membrane comes off easily, and its reason is because the upper layer filtering membrane does not have vitrified bond, causes between rete, intergranular bad adhesion.
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from know-why of the present invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (8)
1. the preparation method of a composite silicon carbide ceramic filter membrane material is characterized in that, its step is following:
1), silit, vitrified bond, pore-forming material and carboxymethyl cellulose being received solution, to receive the mass ratio of solution by silit, vitrified bond, pore-forming material and carboxymethyl cellulose be that the mixed of 10:0.5～3.3:0.5～4.0:1.0～3.0 back that stirs is dry-pressing formed; Obtain carborundum porous ceramics supporter base substrate; Pressure is 10～100MPa, and wherein to receive the mass concentration of solution be 1wt%～4wt% to carboxymethyl cellulose;
Said pore-forming material is a gac, and its grain diameter is 0.1～5 μ m;
2), on carborundum porous ceramics supporter billet surface, be coated with shop one deck sintering volatilizable spackling powder and dry-pressing formed, pressure is 1～5MPa;
3), the equal length of making even is the mullite fiber of 10mm, is that the mixed of 1:0.3～1.5 stirs and obtains the ceramic fiber compound by the mass ratio of mullite fiber, vitrified bond; The ceramic fiber transition layer evenly is coated with is layered on step 2) on the gained section bar surface, and dry-pressing formed, pressure is 1～5 MPa;
4), the mass ratio by sic powder, vitrified bond is the mixed of 10:0.5～3.3 and stirs; Obtain the filtering membrane compound; The filtering membrane compound evenly is coated with is layered on the step 3) gained section bar surface, and dry-pressing formed, and pressure is 1～5 MPa;
5), step 4) gained section bar is carried out sintering, sintering temperature is 1100～1500
oC, temperature rise rate 1～10
oC/min, soaking time is 1～3h, gets the composite silicon carbide ceramic filter membrane material.
2. the preparation method of composite silicon carbide ceramic filter membrane material according to claim 1 is characterized in that: said vitrified bond is that the quartzy mixing and ball milling configuration of 65wt% potassium felspar sand, 12wt% kaolin and 23wt% forms by massfraction.
3. the preparation method of composite silicon carbide ceramic filter membrane material according to claim 2 is characterized in that: the grain diameter of said vitrified bond powder is 0.1～3 μ m.
4. the preparation method of composite silicon carbide ceramic filter membrane material according to claim 1 is characterized in that: the particle diameter at silit described in the step 1) is 180～350 μ m.
5. the preparation method of composite silicon carbide ceramic filter membrane material according to claim 1 is characterized in that: said spackling powder diameter is 0.1～5 μ m.
6. the preparation method of composite silicon carbide ceramic filter membrane material according to claim 1 is characterized in that: said spackling is gac or graphite.
7. the preparation method of composite silicon carbide ceramic filter membrane material according to claim 1 is characterized in that: single diameter Distribution 1～15 μ m of said mullite fiber, length-to-diameter ratio is greater than 10.
8. the preparation method of composite silicon carbide ceramic filter membrane material according to claim 1 is characterized in that: in the filtering membrane compound, add pore-forming material, the massfraction of the pore-forming material that is added is below 30wt%.
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