CN111804159A - Silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting and preparation method thereof - Google Patents
Silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting and preparation method thereof Download PDFInfo
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- CN111804159A CN111804159A CN202010652140.2A CN202010652140A CN111804159A CN 111804159 A CN111804159 A CN 111804159A CN 202010652140 A CN202010652140 A CN 202010652140A CN 111804159 A CN111804159 A CN 111804159A
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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Abstract
The invention relates to a silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting and a preparation method thereof. The separation membrane sequentially comprises a silicon carbide support body, a silicon carbide whisker transition layer and a silicon carbide tape casting separation layer from inside to outside. The raw materials of the silicon carbide support body comprise silicon carbide particles I, silicon carbide whiskers, a dispersing agent and a bonding agent; the raw materials of the silicon carbide flow whisker transition layer comprise silicon carbide whiskers, a dispersing agent and a bonding agent; the raw materials of the silicon carbide tape-casting piece separation layer comprise silicon carbide particles II, silicon carbide whiskers, a bonding agent and a dispersing agent. The silicon carbide whisker reinforced silicon carbide ceramic separation membrane prepared by the invention is composed of pure-phase silicon carbide and does not contain any low-melting-point oxide, so that the membrane has strong chemical corrosion resistance and high-temperature corrosion resistance, and can be used for treating strong-corrosion water bodies and high-temperature water bodies.
Description
Technical Field
The invention belongs to the technical field of inorganic membrane preparation, relates to a silicon carbide ceramic membrane and a preparation method thereof, and particularly relates to a silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting and a preparation method thereof.
Background
The water content of crude oil is high in the process of oil field exploitation, and a large amount of oily sewage is generated after oil-water separation. In addition, most of the produced water in the oil field is treated and then re-injected into the stratum, so that the water source for water injection is solved and the environment is protected. However, the produced water from oil fields contains a large amount of emulsified oil, soluble organic substances, solid particles, inorganic ions, bacteria and the like, and is difficult to separate by a general physical method or a chemical method, and the requirements of water quality discharge and reinjection water are difficult to meet
In recent years, the research and application of ceramic membranes in the treatment of oily wastewater are increasingly considered. The ceramic membrane has the characteristics of high temperature resistance (from room temperature to 1000 ℃), chemical corrosion resistance (the pH value is 1-14), good mechanical strength, strong biological resistance, large permeation quantity, strong cleanability, long service life and the like, and has better separation effect and cleaning recovery. Currently common inorganic ceramic membranes include alumina, zirconia, silica, mullite, and the like. However, the commercial ceramic micro-filtration membranes of alumina, zirconia and the like have a plurality of technical key problems in oil-water separation, mainly including low stable filtration permeation flux, poor membrane anti-pollution capability and high oil content concentration in filtration permeate. Compared with the ceramic membrane of alumina and zirconia, the silicon carbide ceramic membrane has higher porosity, larger membrane flux and stronger chemical stability and high temperature resistance, thus being the first choice of the membrane material for the new generation of sewage treatment in the water treatment industry. Particularly, the wetting angle of the silicon carbide film with water is extremely small, so that the silicon carbide film has better hydrophilicity and lipophobicity; the high hydrophilicity and lipophobicity are the primary factors that the ceramic membrane can have high membrane flux and strong oil pollution resistance in oil-water separation. Therefore, the silicon carbide film has a stronger resistance to oil contamination than aluminum oxide films and other organic films.
Disclosure of Invention
The invention aims to provide a pure-phase silicon carbide ceramic separation membrane with high strength, long service life and high precision.
The above object of the present invention is achieved by the following scheme: the utility model provides a carborundum whisker reinforces carborundum ceramic separation membrane based on curtain coating shaping, the separation membrane include carborundum supporter, carborundum whisker transition layer and by the carborundum curtain coating piece separation layer that constitutes based on the fashioned carborundum whisker of curtain coating from inside to outside in proper order.
In the silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting, the thickness of the silicon carbide whisker transition layer is 1-10 μm.
In the silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting, the thickness of the separation layer of the silicon carbide tape casting sheet is 0.1-1 mm.
In the silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting, the raw material of the silicon carbide support body comprises silicon carbide particles I, silicon carbide whiskers, a dispersing agent and a bonding agent; the raw materials of the silicon carbide flow whisker transition layer comprise silicon carbide whiskers, a dispersing agent and a bonding agent; the raw materials of the silicon carbide tape-casting piece separation layer comprise silicon carbide particles II, silicon carbide whiskers, a bonding agent and a dispersing agent.
In the invention, the silicon carbide whisker has higher rigidity, the densification of the silicon carbide particles I is inhibited by the bridging effect of the whisker in the sintering process, and the silicon carbide particles I and the silicon carbide whisker act together to form more open air holes in the supporter, thereby improving the permeability of the supporter; in addition, the silicon carbide whisker has high fracture strength, and can improve the fracture strength of the support, so that the thickness of the support is reduced. The thickness of the support body in the silicon carbide whisker reinforced silicon carbide ceramic separation membrane is 2-4mm, while the thickness of the support body in the prior art is generally 4-6 mm. The ceramic membrane meets the requirements of high permeability and high strength of the support body. In the silicon carbide whisker reinforced silicon carbide film, silicon carbide particles II and silicon carbide whiskers are selected as raw materials, and the silicon carbide whiskers have higher rigidity, so that the film shrinkage in the drying and firing processes can be inhibited, and the film cracking is reduced.
Preferably, the raw materials of the silicon carbide support body comprise 100 parts of silicon carbide particles I, 20-40 parts of silicon carbide whiskers, 3-5 parts of a dispersing agent and 10-15 parts of a binding agent.
Preferably, the raw materials of the silicon carbide whisker transition layer comprise 100 parts of silicon carbide whiskers, 10-20 parts of a dispersing agent and 10-30 parts of a bonding agent.
Preferably, the raw materials of the silicon carbide tape-casting piece separation layer comprise 100 parts of silicon carbide particles II, 5-10 parts of silicon carbide whiskers, 5-10 parts of a dispersing agent and 10-20 parts of a binding agent.
More preferably, the dispersant is polyvinyl alcohol or polyethylene glycol.
Preferably, the binding agent is sodium carboxymethyl cellulose, the molecular weight of the sodium carboxymethyl cellulose is 10000-16000, and the purity is more than 98%.
Further preferably, the silicon carbide particles I have an average particle size of 3-30 μm and a purity of more than 99%.
More preferably, the silicon carbide particles II have a diameter of 0.1 to 1 μm.
More preferably, the silicon carbide whisker has an aspect ratio of 2 to 5, a diameter of 0.5 to 2 μm, and a length of 3 to 10 μm.
The invention also provides a preparation method of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting, which is characterized by comprising the following steps of:
weighing silicon carbide particles I, silicon carbide whiskers, a dispersing agent and a binding agent, mixing, pugging, ageing and then extruding and molding to obtain a silicon carbide support body biscuit, and sintering the silicon carbide support body biscuit to obtain a silicon carbide support body;
weighing silicon carbide whiskers, a dispersing agent and a bonding agent, mixing to obtain silicon carbide whisker slurry, and spraying the silicon carbide whisker slurry onto the surface of a silicon carbide support to form a silicon carbide whisker transition layer;
weighing silicon carbide particles II, silicon carbide whiskers, a binding agent and a dispersing agent, mixing the silicon carbide particles II, the silicon carbide whiskers, the binding agent and the dispersing agent with deionized water, carrying out ball milling to obtain mud, transferring the mud into a casting machine, carrying out casting molding to obtain silicon carbide cast pieces, and flatly paving the silicon carbide cast pieces on the surface of a silicon carbide support to obtain a semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane;
and (4) transferring the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane into a vacuum sintering furnace, and sintering at high temperature to obtain a silicon carbide whisker reinforced silicon carbide ceramic membrane finished product.
In the preparation process of the silicon carbide whisker reinforced silicon carbide film layer, the solid content of the pug is 40-70%; the thickness of the silicon carbide tape-casting piece is 0.1-1 mm.
In the preparation method of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting, a biscuit of a silicon carbide support body is firstly subjected to heat preservation for 0.5-2 hours at the temperature of 600-800 ℃, then is continuously heated to 1900-2200 ℃, and is subjected to heat preservation for 1-3 hours, so that the silicon carbide support body is obtained.
In the preparation method of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting molding, the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane is moved into a vacuum sintering furnace, and is firstly subjected to heat preservation for 0.5-1 h at the temperature of 600-800 ℃, and then is continuously heated to 1500-1800 ℃ and is subjected to heat preservation for 1-2h, so that a finished product of the silicon carbide whisker reinforced silicon carbide ceramic membrane is obtained.
Compared with the prior art, the silicon carbide whisker reinforced silicon carbide ceramic separation membrane prepared by the invention is composed of pure-phase silicon carbide and does not contain any low-melting-point oxide, so that the silicon carbide whisker reinforced silicon carbide ceramic separation membrane has stronger chemical corrosion resistance and high-temperature corrosion resistance, and can be used for treating strong-corrosion water bodies and high-temperature water bodies. The prepared supporter is prepared from silicon carbide particles and silicon carbide whiskers, and the porosity and the breaking strength of the supporter are improved by adding the silicon carbide whiskers; the silicon carbide whisker transition layer is paved between the support body and the membrane layer, so that the residual stress in the interface is reduced, the membrane layer is prevented from cracking and falling off, the aperture difference between the support body and the membrane layer is reduced, and the service life of the ceramic membrane is prolonged; the film layer is formed by sintering silicon carbide tape-casting sheets, has the characteristics of uniform thickness and convenient preparation, and a small amount of silicon carbide whiskers are added into the film layer, so that the cracking of the film layer in the drying and sintering processes is reduced, and the integrity of the film layer is improved.
Drawings
FIG. 1 is a schematic view showing the structure of a silicon carbide ceramic separation membrane according to the present invention.
FIG. 2 is a diagram showing the morphology of silicon carbide whiskers in the silicon carbide ceramic separation membrane of the present invention.
In the figure, 1, a silicon carbide support; 2. a silicon carbide whisker transition layer; 3. and (3) separating the silicon carbide tape-casting sheet.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1
Weighing 100 parts of silicon carbide particles I, 30 parts of silicon carbide whiskers, 4 parts of dispersing agent and 12 parts of binding agent, respectively stirring and dissolving the dispersing agent and the binding agent in a proper amount of warm water, then sequentially adding the silicon carbide particles I and the silicon carbide whiskers, and uniformly mixing by using a high-speed mixer; and (3) pugging and aging the uniformly mixed pug, extruding and molding to obtain a biscuit of the silicon carbide support body, drying the biscuit, transferring the biscuit into a vacuum sintering furnace, preserving heat at 700 ℃ for 1.2h, continuously heating to 2050 ℃, and preserving heat for 2h to obtain the silicon carbide support body.
Weighing 100 parts of silicon carbide whisker, 15 parts of dispersing agent and 20 parts of bonding agent, respectively stirring and dissolving the dispersing agent and the bonding agent in warm water, then adding the silicon carbide whisker, and uniformly mixing by using a high-speed mixer to obtain silicon carbide whisker slurry; and spraying the silicon carbide whisker slurry on the surface of the silicon carbide support.
Weighing 100 parts of silicon carbide particles II, 8 parts of silicon carbide whiskers, 8 parts of a dispersing agent and 15 parts of a binding agent, mixing the silicon carbide particles II, the silicon carbide whiskers, the binding agent and the dispersing agent with deionized water, and then carrying out ball milling to obtain uniform pug with the solid content of 50%; transferring the pug into a casting machine, and carrying out casting molding to obtain a silicon carbide cast piece separation layer; and drying, shaping and cutting the casting sheet, and then spreading the casting sheet on the surface of the silicon carbide support (actually the surface of the transition layer of the silicon carbide whisker) to obtain the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane. The average grain diameter of the silicon carbide particles I is 20 mu m, and the purity is more than 99 percent; the average diameter of the silicon carbide crystal whisker is 1 μm, and the average length is 5 μm; the silicon carbide particles II had a diameter of 0.5. mu.m. The dispersant is polyvinyl alcohol, and the binder is sodium carboxymethylcellulose with a molecular weight of 12000 and a purity of more than 98%.
And transferring the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane into a vacuum sintering furnace, preserving heat for 0.8h at 700 ℃, continuously heating to 1700 ℃, and preserving heat for 1.5h to obtain the finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane. The thickness of the silicon carbide whisker transition layer is 8 mu m; the thickness of the silicon carbide cast sheet separation layer was 0.5 mm. The thickness of the prepared silicon carbide support body is 2mm, the breaking strength of the silicon carbide support body is 56MPa, and the average pore diameter is 5 mu m. The filtration precision of the prepared silicon carbide ceramic separation membrane finished product is 0.4 mu m, and the pure water flux is 2300L/(m)2H) (pressure difference 0.2 bar).
Example 2
Weighing 100 parts of silicon carbide particles I, 25 parts of silicon carbide whiskers, 4 parts of a dispersing agent and 14 parts of a binding agent, respectively stirring and dissolving the dispersing agent and the binding agent in a proper amount of warm water, then sequentially adding the silicon carbide particles I and the silicon carbide whiskers, and uniformly mixing by using a high-speed mixer; and (3) pugging and aging the uniformly mixed pug, extruding and molding to obtain a biscuit of the silicon carbide support body, drying the biscuit, transferring the biscuit into a vacuum sintering furnace, preserving heat at 650 ℃ for 1.5 hours, then continuously heating to 2000 ℃, and preserving heat for 2 hours to obtain the silicon carbide support body.
Weighing 100 parts of silicon carbide whisker, 12 parts of dispersing agent and 26 parts of binding agent, respectively stirring and dissolving the dispersing agent and the binding agent in warm water, then adding the silicon carbide whisker, and uniformly mixing by using a high-speed mixer to obtain silicon carbide whisker slurry; and spraying the silicon carbide whisker slurry on the surface of the silicon carbide support.
Weighing 100 parts of silicon carbide particles II, 8 parts of silicon carbide whiskers, 6 parts of dispersing agent and 18 parts of binding agent, mixing the silicon carbide particles II, the silicon carbide whiskers, the binding agent and the dispersing agent with deionized water, and then carrying out ball milling to obtain uniform pug with the solid content of 40%; transferring the pug into a casting machine, and carrying out casting molding to obtain a silicon carbide cast piece separation layer; and drying, shaping and cutting the casting sheet, and then spreading the casting sheet on the surface of the silicon carbide support (actually the surface of the transition layer of the silicon carbide whisker) to obtain the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane. The average grain diameter of the silicon carbide particles I is 20 mu m, and the purity is more than 99 percent; the average diameter of the silicon carbide crystal whisker is 1.5 mu m, and the average length of the silicon carbide crystal whisker is 9 mu m; the silicon carbide particles II have a diameter of 0.5. mu.m. The dispersant is polyvinyl alcohol, and the binder is sodium carboxymethylcellulose with a molecular weight of 12000 and a purity of more than 98%.
And transferring the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane into a vacuum sintering furnace, preserving heat for 0.6h at 750 ℃, continuously heating to 1750 ℃, and preserving heat for 1.6h to obtain the finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane. The thickness of the silicon carbide whisker transition layer is 10 mu m; the thickness of the silicon carbide cast sheet separation layer was 0.7 mm. The thickness of the prepared silicon carbide support body is 2.5mm, the breaking strength of the silicon carbide support body is 59MPa, and the average pore diameter is 4.5 mu m. The filtration precision of the prepared silicon carbide ceramic separation membrane finished product is 0.4 mu m, and the pure water flux is 2200L/(m)2H) (pressure difference 0.2 bar).
Example 3
Weighing 100 parts of silicon carbide particles I, 20 parts of silicon carbide whiskers, 5 parts of dispersing agent and 10 parts of binding agent, respectively stirring and dissolving the dispersing agent and the binding agent in a proper amount of warm water, then sequentially adding the silicon carbide particles I and the silicon carbide whiskers, and uniformly mixing by using a high-speed mixer; and (3) pugging and aging the uniformly mixed pug, extruding and molding to obtain a biscuit of the silicon carbide support body, drying the biscuit, transferring the biscuit into a vacuum sintering furnace, preserving heat at 600 ℃ for 2 hours, then continuously heating to 1900 ℃, and preserving heat for 3 hours to obtain the silicon carbide support body.
Weighing 100 parts of silicon carbide whisker, 20 parts of dispersing agent and 10 parts of binding agent, respectively stirring and dissolving the dispersing agent and the binding agent in warm water, then adding the silicon carbide whisker, and uniformly mixing by using a high-speed mixer to obtain silicon carbide whisker slurry; and spraying the silicon carbide whisker slurry on the surface of the ceramic support.
Weighing 100 parts of silicon carbide particles II, 10 parts of silicon carbide whiskers, 5 parts of a dispersing agent and 20 parts of a binding agent, mixing the silicon carbide particles II, the silicon carbide whiskers and the dispersing agent with deionized water, and then carrying out ball milling to obtain uniform pug with solid content of 45%; transferring the pug into a casting machine, and carrying out casting molding to obtain a silicon carbide cast piece separation layer; and drying, shaping and cutting the casting sheet, and then flatly paving the casting sheet on the surface of the ceramic support (actually the surface of the transition layer of the silicon carbide whisker) to obtain the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane. The average grain diameter of the silicon carbide particles I is 10 mu m, and the purity is more than 99 percent; the average diameter of the silicon carbide crystal whisker is 0.5 μm, and the average length is 3 μm; the silicon carbide particles II have a diameter of 0.5. mu.m. The dispersant is polyethylene glycol, and the binder is sodium carboxymethylcellulose with a molecular weight of 12000 and a purity of more than 98%.
And transferring the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane into a vacuum sintering furnace, preserving heat for 1h at 600 ℃, continuously heating to 1800 ℃, and preserving heat for 1h to obtain the finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane. The thickness of the silicon carbide whisker transition layer is 8 mu m; the thickness of the silicon carbide cast sheet separation layer was 0.7 mm. The thickness of the prepared silicon carbide support body is 3mm, the breaking strength of the silicon carbide support body is 67MPa, and the average pore diameter is 3 mu m. The filtration precision of the prepared silicon carbide ceramic separation membrane finished product is 0.25 mu m, and the pure water flux is 1500L/(m)2H) (pressure difference 0.2 bar).
Example 4
Weighing 100 parts of silicon carbide particles I, 40 parts of silicon carbide whiskers, 3 parts of dispersing agent and 15 parts of binding agent, respectively stirring and dissolving the dispersing agent and the binding agent in a proper amount of warm water, then sequentially adding the silicon carbide particles I and the silicon carbide whiskers, and uniformly mixing by using a high-speed mixer; and (3) pugging and aging the uniformly mixed pug, then extruding and molding to obtain a biscuit of the silicon carbide support body, drying the biscuit, then transferring the biscuit into a vacuum sintering furnace, preserving heat at 800 ℃ for 0.5h, then continuously heating to 2200 ℃ and preserving heat for 1h to obtain the silicon carbide support body.
Weighing 100 parts of silicon carbide whisker, 10 parts of dispersing agent and 30 parts of binding agent, respectively stirring and dissolving the dispersing agent and the binding agent in warm water, then adding the silicon carbide whisker, and uniformly mixing by using a high-speed mixer to obtain silicon carbide whisker slurry; and spraying the silicon carbide whisker slurry on the surface of the ceramic support.
Weighing 100 parts of silicon carbide particles II, 5 parts of silicon carbide whiskers, 10 parts of a dispersing agent and 10 parts of a binding agent, mixing the silicon carbide particles II, the silicon carbide whiskers, the binding agent and the dispersing agent with deionized water, and then carrying out ball milling to obtain uniform pug with solid content of 60%; transferring the pug into a casting machine, and carrying out casting molding to obtain a silicon carbide cast piece separation layer; and drying, shaping and cutting the casting sheet, and then flatly paving the casting sheet on the surface of the ceramic support (actually the surface of the transition layer of the silicon carbide whisker) to obtain the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane. The average grain diameter of the silicon carbide particles I is 20 mu m, and the purity is more than 99 percent; the average length-diameter ratio of the silicon carbide crystal whisker is 5, the average diameter is 2 mu m, and the average length is 10 mu m; the silicon carbide particles II had a diameter of 0.3. mu.m. The dispersant is polyethylene glycol, and the binder is sodium carboxymethylcellulose with molecular weight of 15000 and purity of more than 98%.
And transferring the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane into a vacuum sintering furnace, preserving heat for 0.5h at 800 ℃, continuously heating to 1500 ℃, and preserving heat for 1h to obtain the finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane. The thickness of the silicon carbide whisker transition layer is 8 mu m; the thickness of the silicon carbide cast sheet separation layer was 0.8 mm. The thickness of the prepared silicon carbide support body is 2mm, the breaking strength of the silicon carbide support body is 65MPa, and the average pore diameter is 3.8 mu m. The filtration precision of the prepared silicon carbide ceramic separation membrane finished product is 0.3 mu m, and the pure water flux is 1800L/(m)2H) (pressure difference 0.2 bar).
Example 5
The difference from example 1 is that silicon carbide particles I are used in both ceramic membrane support and silicon carbide cast sheet in this example, i.e. silicon carbide particles II are not used in silicon carbide cast sheet, and the other steps are the same as in the example and will not be described again here. The breaking strength of the prepared silicon carbide support body is 56MPa, and the average pore diameter is 5 mu m. The prepared silicon carbide ceramic separation membrane finished productThe filtration precision is 4.5 μm, and the pure water flux is about 200000L/(m)2H) (pressure difference 0.2 bar).
Example 6
The difference from example 1 is that silicon carbide particles II are used in both ceramic membrane support and silicon carbide cast sheet in this example, i.e. silicon carbide particles I are not used in silicon carbide cast sheet, and the other steps are the same as in the example and will not be described again here. The breaking strength of the prepared silicon carbide support is 124MPa, and the average pore diameter is 0.5 mu m. The filtration precision of the prepared silicon carbide ceramic separation membrane finished product is 0.4 mu m, and the pure water flux is 1500L/(m)2H) (pressure difference 0.2 bar).
Example 7
The difference from example 1 is that there are no silicon carbide whiskers in both the ceramic membrane support and the silicon carbide cast sheet in this example, and the other steps are the same as in the example, and will not be described again here. The breaking strength of the prepared silicon carbide support body is 48MPa, and the average pore diameter is 3.5 mu m. The filtration precision of the prepared silicon carbide ceramic separation membrane finished product is 0.3 mu m, and the pure water flux is 2000L/(m)2H) (pressure difference 0.2 bar).
Example 8
The difference from example 1 is that the ceramic membrane support in this example is free of silicon carbide whiskers, and the rest is the same as the example and will not be described again here. The breaking strength of the prepared silicon carbide support body is 53MPa, and the average pore diameter is 4 mu m. The filtration precision of the prepared silicon carbide ceramic separation membrane finished product is 0.4 mu m, and the pure water flux is 2300L/(m)2H) (pressure difference 0.2 bar).
Example 9
The difference from example 1 is only that there are no silicon carbide whiskers in the separation layer of the silicon carbide cast sheet in this example, and the other steps are the same as in the example and will not be repeated here. The breaking strength of the prepared silicon carbide support body is 56MPa, and the average pore diameter is 5 mu m. The filtration precision of the prepared silicon carbide ceramic separation membrane finished product is 0.3 mu m, and the pure water flux is 2100L/(m)2H) (pressure difference 0.2 bar).
Comparative example 1
The only difference from example 1 is that this comparative example does not contain silicon carbide whiskersThe transition layer was composed of only the silicon carbide support and the silicon carbide cast piece separation layer as in example 1. The breaking strength of the prepared silicon carbide support body is 56MPa, and the average pore diameter is 4 mu m. The filtration precision of the prepared silicon carbide ceramic separation membrane finished product is 0.4 mu m, and the pure water flux is 2150L/(m)2H) (pressure difference 0.2 bar).
The technical scope of the invention claimed by the embodiments herein is not exhaustive and new solutions formed by equivalent replacement of single or multiple technical features in the embodiments are also within the scope of the invention, and all parameters involved in the solutions of the invention do not have mutually exclusive combinations if not specifically stated.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (10)
1. The silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting is characterized by sequentially comprising a silicon carbide support body, a silicon carbide whisker transition layer and a silicon carbide tape casting sheet separation layer from inside to outside.
2. The silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting according to claim 1, wherein the thickness of the silicon carbide whisker transition layer is 1 to 10 μm.
3. The cast silicon carbide whisker reinforced silicon carbide ceramic separation membrane of claim 1, wherein the thickness of the cast sheet layer of silicon carbide is 0.1-1 mm.
4. The silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting according to claim 1, wherein the raw material of the silicon carbide support comprises silicon carbide particles I, silicon carbide whiskers, a dispersing agent and a binder;
the raw materials of the silicon carbide flow whisker transition layer comprise silicon carbide whiskers, a dispersing agent and a bonding agent;
the raw materials of the silicon carbide tape-casting piece separation layer comprise silicon carbide particles II, silicon carbide whiskers, a bonding agent and a dispersing agent.
5. The silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting according to claim 4, wherein the silicon carbide particles I have an average particle size of 3 to 30 μm and a purity of more than 99%.
6. The silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting according to claim 4, wherein the silicon carbide particles II have a diameter of 0.1 to 1 μm.
7. The silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on cast molding according to claim 4, wherein the silicon carbide whiskers have an aspect ratio of 2 to 5, a diameter of 0.5 to 2 μm, and a length of 3 to 10 μm.
8. A method for preparing a silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting according to claim 1, comprising the steps of:
weighing silicon carbide particles I, silicon carbide whiskers, a dispersing agent and a binding agent, mixing, pugging, ageing and then extruding and molding to obtain a silicon carbide support body biscuit, and sintering the silicon carbide support body biscuit to obtain a silicon carbide support body;
weighing silicon carbide whiskers, a dispersing agent and a bonding agent, mixing to obtain silicon carbide whisker slurry, and spraying the silicon carbide whisker slurry onto the surface of a silicon carbide support to form a silicon carbide whisker transition layer;
weighing silicon carbide particles II, silicon carbide whiskers, a binding agent and a dispersing agent, mixing the silicon carbide particles II, the silicon carbide whiskers, the binding agent and the dispersing agent with deionized water, carrying out ball milling to obtain mud, transferring the mud into a casting machine, carrying out casting molding to obtain silicon carbide cast pieces, and flatly paving the silicon carbide cast pieces on the surface of a silicon carbide support to obtain a semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane;
and transferring the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane into a vacuum sintering furnace, and sintering at high temperature to obtain the finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane.
9. The preparation method of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting according to claim 8, wherein the ceramic membrane support is obtained by first preserving heat of a biscuit of a silicon carbide support at 600-800 ℃ for 0.5-2 h, then continuously heating to 1900-2200 ℃ and preserving heat for 1-3 h.
10. The preparation method of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane based on tape casting according to claim 8, wherein the semi-finished product of the silicon carbide whisker reinforced silicon carbide ceramic separation membrane is moved into a vacuum sintering furnace, and is subjected to heat preservation at 600-800 ℃ for 0.5-1 h, then is continuously heated to 1500-1800 ℃ and is subjected to heat preservation for 1-2h, so as to obtain the finished product of the silicon carbide whisker reinforced silicon carbide ceramic membrane.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113800946A (en) * | 2021-10-08 | 2021-12-17 | 雅安沃克林环保科技有限公司 | Preparation process of ceramic membrane and co-extrusion die |
| CN115044842A (en) * | 2021-06-24 | 2022-09-13 | 珠海亿特立新材料有限公司 | Production system for preparing high-specific-rigidity aluminum silicon carbide structural part |
| CN115253724A (en) * | 2022-08-09 | 2022-11-01 | 武汉工程大学 | Silicon carbide ceramic nanowire gridding nanofiltration membrane separation layer and preparation method thereof |
| CN116283300A (en) * | 2023-03-17 | 2023-06-23 | 山东理工大学 | Digital light processing-based one-step cofiring silicon carbide flat ceramic membrane and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113110A (en) * | 2012-12-04 | 2013-05-22 | 海南大学 | Application method of composite silicon carbide ceramic fiber transition layer |
| CN105727755A (en) * | 2014-12-09 | 2016-07-06 | 中国科学院金属研究所 | Gradient-pore silicon nitride and silicon carbide combined film tube and preparation method therefor |
| CN107663088A (en) * | 2017-08-03 | 2018-02-06 | 浙江理工大学 | A kind of preparation method of low-temperature sintering acid and alkali-resistance porous silicon carbide ceramic film |
| CN108261928A (en) * | 2018-01-26 | 2018-07-10 | 山东理工大学 | Pure silicon carbide ceramics membrane component and preparation method thereof |
| CN108686524A (en) * | 2018-05-08 | 2018-10-23 | 武汉工程大学 | The preparation method of the silicon carbide ceramics hollow-fibre membrane of silicon carbide whisker strengthening and toughening |
-
2020
- 2020-07-08 CN CN202010652140.2A patent/CN111804159B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103113110A (en) * | 2012-12-04 | 2013-05-22 | 海南大学 | Application method of composite silicon carbide ceramic fiber transition layer |
| CN105727755A (en) * | 2014-12-09 | 2016-07-06 | 中国科学院金属研究所 | Gradient-pore silicon nitride and silicon carbide combined film tube and preparation method therefor |
| CN107663088A (en) * | 2017-08-03 | 2018-02-06 | 浙江理工大学 | A kind of preparation method of low-temperature sintering acid and alkali-resistance porous silicon carbide ceramic film |
| CN108261928A (en) * | 2018-01-26 | 2018-07-10 | 山东理工大学 | Pure silicon carbide ceramics membrane component and preparation method thereof |
| CN108686524A (en) * | 2018-05-08 | 2018-10-23 | 武汉工程大学 | The preparation method of the silicon carbide ceramics hollow-fibre membrane of silicon carbide whisker strengthening and toughening |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115044842A (en) * | 2021-06-24 | 2022-09-13 | 珠海亿特立新材料有限公司 | Production system for preparing high-specific-rigidity aluminum silicon carbide structural part |
| CN113800946A (en) * | 2021-10-08 | 2021-12-17 | 雅安沃克林环保科技有限公司 | Preparation process of ceramic membrane and co-extrusion die |
| CN113800946B (en) * | 2021-10-08 | 2022-11-11 | 雅安沃克林环保科技有限公司 | Preparation process of ceramic membrane and co-extrusion die |
| CN115253724A (en) * | 2022-08-09 | 2022-11-01 | 武汉工程大学 | Silicon carbide ceramic nanowire gridding nanofiltration membrane separation layer and preparation method thereof |
| CN115253724B (en) * | 2022-08-09 | 2024-05-31 | 武汉工程大学 | Silicon carbide ceramic nanowire mesh nanofiltration membrane separation layer and preparation method thereof |
| CN116283300A (en) * | 2023-03-17 | 2023-06-23 | 山东理工大学 | Digital light processing-based one-step cofiring silicon carbide flat ceramic membrane and preparation method thereof |
| CN116283300B (en) * | 2023-03-17 | 2024-05-17 | 山东理工大学 | Digital light processing-based one-step cofiring silicon carbide flat ceramic membrane and preparation method thereof |
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