CN114311232B - Preparation method of large-diameter combined honeycomb ceramic filter membrane - Google Patents
Preparation method of large-diameter combined honeycomb ceramic filter membrane Download PDFInfo
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- CN114311232B CN114311232B CN202011056922.6A CN202011056922A CN114311232B CN 114311232 B CN114311232 B CN 114311232B CN 202011056922 A CN202011056922 A CN 202011056922A CN 114311232 B CN114311232 B CN 114311232B
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Abstract
The invention discloses a preparation method of a large-diameter combined honeycomb ceramic filter membrane, which comprises the following steps: (1) Preparing blank body pug, and ageing to obtain aged pug; (2) Extruding the stale pug by an extruder to form a blank body with a sector-shaped cross section, rapidly cooling the blank body to 0-5 ℃ in 20-35s by using low-temperature nitrogen at a die opening of the extruder while extruding, and cutting the blank body after extruding to a set length to obtain a high-strength blank body; (3) Freeze-drying the high-strength green body, and sintering to obtain a honeycomb ceramic membrane support body; (4) Preparing at least one filter membrane layer on the honeycomb ceramic membrane support body to obtain a ceramic membrane component; (5) And assembling the ceramic membrane components according to a set interval to form the large-diameter combined honeycomb ceramic filter membrane with a circular cross section. The invention has low molding pressure, small abrasion to extrusion equipment and dies, no deformation and cracking of the blank body and high yield of 93-98%.
Description
Technical Field
The invention belongs to the technical field of ceramic membranes, and particularly relates to a preparation method of a large-diameter combined honeycomb ceramic filter membrane.
Background
Inorganic ceramic membranes are increasingly widely used in the fields of oil-water separation, water treatment and the like due to the characteristics of high strength, strong corrosion resistance, stable structure, no microbial corrosion, uniform pore size distribution and the like. The ceramic membranes applied to the water treatment industry at present mainly have various configurations such as flat ceramic membranes, disc type ceramic membranes, small-diameter tubular ceramic membranes, honeycomb ceramic membranes, hollow fiber ceramic membranes and the like.
Among ceramic membranes with various configurations, the large-diameter honeycomb ceramic membrane has the characteristics of large filling area, low unit membrane cost, high strength, simple components, long service life and the like, and is an ideal configuration for applying the ceramic membrane to water treatment. At present, the mainstream honeycomb ceramic membrane in the market is mainly a tubular honeycomb ceramic membrane which is extruded and molded at one time and is processed with a channel for measuring accumulated water. However, because the large-diameter honeycomb ceramic membrane has a large number of through holes and high hole density, kong Bibao, the green body is heavy in weight, and the green body is very easy to deform in the forming process, easy to crack, large in equipment and mold loss, low in yield and high in preparation cost. In order to improve the water outlet efficiency of the water treatment honeycomb ceramic membrane in the operation process, a water accumulation flow channel needs to be processed on the side surface of the honeycomb ceramic membrane after the honeycomb ceramic membrane is biscuit-fired or sintered. In the accumulated water flow passage processing process, the honeycomb ceramic membrane has high hardness, large brittleness, high processing cost and easy cracking, so that the yield and the preparation cost of the honeycomb ceramic membrane are further reduced. CN209034121U discloses an annular ceramic membrane element and a honeycomb ceramic membrane module containing the same, which combines a group of large-diameter honeycomb ceramic membranes by using a plurality of annular ceramic membrane tubes with different diameters. However, the annular honeycomb ceramic membrane tube with the structure has a hollow structure, has no internal supporting structure, and also has the problems of easy deformation and cracking, low yield, need of multiple sets of dies and high preparation cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a large-diameter combined honeycomb ceramic filter membrane.
The technical scheme of the invention is as follows:
a preparation method of a large-diameter combined honeycomb ceramic filter membrane comprises the following steps:
(1) Preparing a blank body pug, and ageing to obtain an aged pug; the blank pug contains 2-4wt% of gelatin powder and 3-6wt% of hydroxypropyl methylcellulose with the gel temperature of 40-100 ℃;
(2) Extruding the stale pug into a sector blank with the cross section of 0-180 degrees by an extruder at the temperature of 40-100 ℃ and under the extrusion pressure of 5-7MPa, rapidly cooling the blank to 0-5 ℃ within 20-35s by using low-temperature nitrogen while extruding, and cutting after extruding to a set length to obtain a high-strength blank;
(3) Freeze-drying the high-strength green body at-52 to-48 ℃ for 45 to 50 hours, and sintering to obtain a honeycomb ceramic membrane support body;
(4) Preparing at least one filter membrane layer on the honeycomb ceramic membrane support body to obtain a ceramic membrane component;
(5) And assembling at least two ceramic membrane components according to a set interval to form the large-diameter combined honeycomb ceramic filter membrane with a circular cross section, the diameter of 110-130mm and the length of 1.1-1.3m, wherein a gap between adjacent ceramic membrane components is a ponding flow channel.
In a preferred embodiment of the present invention, the green body paste in the step (1) further contains alumina micropowder, silica micropowder, magnesium oxide, tung oil and RO water.
Further preferably, the formula of the green body pug in the step (1) is as follows: 72-74wt% of aluminum oxide micro powder, 1-2wt% of silicon oxide micro powder, 0.8-1.2wt% of magnesium oxide, 0.4-0.6wt% of tung oil, 2-4wt% of gelatin powder, 3-6wt% of hydroxypropyl methyl cellulose and the balance of RO water.
Still more preferably, the formulation of the green body pug in the step (1) is as follows: 73wt% of aluminum oxide micro powder, 1.5wt% of silicon oxide micro powder, 1wt% of magnesium oxide, 0.5wt% of tung oil, 2-4wt% of gelatin powder, 3-6wt% of hydroxypropyl methyl cellulose and the balance of RO water.
In a preferred embodiment of the present invention, the fine alumina powder has a particle size larger than that of the fine silica powder.
More preferably, the particle size of the alumina fine powder is 30 to 40 μm, and the particle size of the silica fine powder is 1.5 to 2.5 μm.
More preferably, the particle size of the alumina fine powder is 35 μm, and the particle size of the silica fine powder is 2 μm.
In a preferred embodiment of the present invention, the temperature of the aging in the step (1) is 50 to 55 ℃ and the time is 72 to 96 hours.
In a preferred embodiment of the present invention, the extrusion speed of the extruder in the step (2) is 0.01 to 0.012m/s.
In a preferred embodiment of the present invention, the sintering temperature in the step (4) is 1745-1750 ℃ and the time is 2.5-3.5h.
The invention has the beneficial effects that:
1. the invention has low molding pressure, small abrasion to extrusion equipment and a die, no deformation and cracking of a green body, high yield of 93-98%, and formation of the honeycomb ceramic filter membrane with a circular cross section by assembling ceramic membrane components according to a set interval without machining a side accumulated water flow passage, thereby greatly improving the yield of the honeycomb ceramic membrane and reducing the preparation cost.
2. In the invention, gelatin is dissolved into colloid in a heating state, and is cooled to below 35-40 ℃ to form gel, hydroxypropyl methyl cellulose with high gel temperature can not be separated out in a high temperature state, has good dispersion water retention property, can be used as a forming auxiliary agent, and the pug in the extrusion process is heated to 40-100 ℃ by using an extruder heating device, so that the pug has good fluidity and is formed under low extrusion pressure.
3. In the invention, the extruded green body is rapidly cooled to 0-5 ℃ at the extrusion port of the extruder by using a low-temperature gas purging mode, and the wet green strength can be instantly improved.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Example 1
Uniformly mixing aluminum oxide micro powder (35 mu m,73 wt%), silicon oxide micro powder (2um, 1.5 wt%), magnesium oxide (1 wt%), tung oil (0.5 wt%), gelatin powder (2 wt%), hydroxypropyl methyl cellulose (gel temperature is 75 ℃,6 wt%) and RO water (16 wt%) at normal temperature to prepare blank pug, and putting the blank pug in a 50 ℃ heat preservation box for ageing for 72 hours to obtain the aged pug. And then extruding and molding the aged pug by using an extruder (the obtained blank is a fan-shaped blank with the cross section of 90 degrees), setting the heating temperature of the extruder to be 50 ℃, the extrusion pressure to be 5.5Mpa and the extrusion speed to be 0.01m/s. And (3) rapidly cooling the green body to 5 ℃ within 20s by adopting low-temperature nitrogen at the die opening of the honeycomb ceramic membrane die of the extruder, extruding the green body with a certain length, and cutting the green body to obtain a high-strength green body. And (3) freeze-drying the high-strength green body at-50 ℃ for 48h, and then sintering at 1750 ℃ for 3h to form the honeycomb ceramic membrane support. And finally, combining the four ceramic membrane components into a large-diameter combined honeycomb ceramic filter membrane product according to a set distance, wherein a gap between every two adjacent ceramic membrane components is a ponding flow channel. The bending degree of the product with the diameter of 120mm and the length of 1.2m prepared by the embodiment is less than 1.5mm, the deviation of the outer diameter is less than 1.2mm, and the yield is 96%.
Example 2
Uniformly mixing aluminum oxide micro powder (35 mu m,73 wt%), silicon oxide micro powder (2um, 1.5 wt%), magnesium oxide (1 wt%), tung oil (0.5 wt%), gelatin powder (4 wt%), hydroxypropyl methyl cellulose (the gel temperature is 75 ℃,3 wt%) and RO water (17 wt%) at normal temperature to prepare blank pug, and putting the blank pug in a 55 ℃ heat preservation box for ageing for 96 hours to obtain the aged pug. And then extruding and molding the aged pug by using an extruder (the obtained blank is a fan-shaped blank with the cross section of 90 degrees of radian), setting the heating temperature of the extruder to be 50 ℃, the extrusion pressure to be 7Mpa and the extrusion speed to be 0.012m/s. And (3) rapidly cooling the green body to 0 ℃ within 35 seconds by adopting low-temperature nitrogen at the die opening of the honeycomb ceramic membrane die of the extruder, extruding the green body with a certain length, and cutting the green body to obtain a high-strength green body. And freeze-drying the high-strength green body at-50 ℃ for 48h, and sintering at 1750 ℃ for 3h to form the honeycomb ceramic membrane support. And finally, combining the four ceramic membrane components into a large-diameter combined honeycomb ceramic filter membrane product according to a set distance, wherein a gap between every two adjacent ceramic membrane components is a ponding flow channel. The bending degree of the product with the diameter of 120mm and the length of 1.2m prepared by the embodiment is less than 2.0mm, the deviation of the outer diameter is less than 1.8mm, and the yield is 94.5%.
Example 3
Uniformly mixing aluminum oxide micro powder (35 mu m,73 wt%), silicon oxide micro powder (2um, 1.5 wt%), magnesium oxide (1 wt%), tung oil (0.5 wt%), gelatin powder (3 wt%), hydroxypropyl methyl cellulose (gel temperature is 75 ℃,5 wt%) and RO water (16 wt%) at normal temperature to prepare blank pug, and putting the blank pug in a 55 ℃ incubator to be aged for 96 hours to obtain aged pug. And then, extruding and molding the aged pug by using an extruder (the obtained blank is a fan-shaped blank with the cross section of 90 degrees), setting the heating temperature of the extruder to be 50 ℃, the extrusion pressure to be 5.1Mpa and the extrusion speed to be 0.011m/s. And (3) rapidly cooling the green body to 2 ℃ within 30s by adopting low-temperature nitrogen at the die opening of the honeycomb ceramic membrane die of the extruder, extruding the green body with a certain length, and cutting the green body to obtain the high-strength green body. And (3) freeze-drying the high-strength green body at-50 ℃ for 48h, and then sintering at 1750 ℃ for 3h to form the honeycomb ceramic membrane support. And finally, combining the four ceramic membrane components into a large-diameter combined honeycomb ceramic filter membrane product according to a set distance, wherein a gap between every two adjacent ceramic membrane components is a ponding flow channel. The bending degree of the product with the diameter of 120mm and the length of 1.2m prepared by the embodiment is less than 1.2mm, the deviation of the outer diameter is less than 1.2mm, and the yield is 98%.
Comparative example 1
Uniformly mixing aluminum oxide micro powder (35 mu m,73 wt%), silicon oxide micro powder (2um, 1.5 wt%), magnesium oxide (1 wt%), tung oil (0.5 wt%), gelatin powder (1 wt%), hydroxypropyl methyl cellulose (the gel temperature is 75 ℃,6 wt%) and RO water (17 wt%) at normal temperature to prepare blank pug, and putting the blank pug in a 50 ℃ heat preservation box for ageing for 72 hours to obtain the aged pug. And then, extruding and molding the aged pug by using an extruder (the obtained blank is a fan-shaped blank with the cross section of 90 degrees), and setting the heating temperature of the extruder to be 50 ℃ and the extrusion pressure to be 11Mpa. And (3) rapidly cooling the green body to 5 ℃ within 30s by adopting low-temperature nitrogen at the die opening of the honeycomb ceramic membrane die of the extruder, extruding the green body with a certain length, and cutting the green body to obtain the high-strength green body. And (3) freeze-drying the high-strength green body at-50 ℃ for 48h, and then sintering at 1750 ℃ for 3h to form the honeycomb ceramic membrane support. And finally, combining the four ceramic membrane components into a large-diameter combined honeycomb ceramic filter membrane product according to a set distance, wherein a gap between every two adjacent ceramic membrane components is a ponding flow channel. The bending degree of the product with the diameter of 120mm and the length of 1.2m prepared by the comparative example is less than 13mm, the deviation of the outer diameter is less than 28mm, and the yield is 40%.
Comparative example 2
Uniformly mixing aluminum oxide micro powder (35 mu m,73 wt%), silicon oxide micro powder (2um, 1.5 wt%), magnesium oxide (1 wt%), tung oil (0.5 wt%), gelatin powder (2 wt%), hydroxypropyl methyl cellulose (gel temperature is 75 ℃,7 wt%) and RO water (15 wt%) at normal temperature to prepare a blank body pug, and putting the blank body pug in a 50 ℃ heat preservation box for ageing for 72 hours to obtain the aged pug. And then extruding and molding the aged pug by using an extruder (the obtained blank is a fan-shaped blank with the cross section of 90 degrees), setting the heating temperature of the extruder to be 50 ℃ and the extrusion pressure to be 5.7Mpa. And (3) rapidly cooling the green body to 5 ℃ within 30s by adopting low-temperature nitrogen at the die opening of the honeycomb ceramic membrane die of the extruder, extruding the green body with a certain length, and cutting the green body to obtain the high-strength green body. The high-strength blank is frozen and dried for 48h at minus 50 ℃ and then sintered for 3h at 1750 ℃ at high temperature, then the membrane tube is cracked, and the qualification rate of the finished product is 0%.
Comparative example 3
Uniformly mixing aluminum oxide micro powder (35 mu m,73 wt%), silicon oxide micro powder (2um, 1.5 wt%), magnesium oxide (1 wt%), tung oil (0.5 wt%), gelatin powder (5 wt%), hydroxypropyl methyl cellulose (gel temperature is 75 ℃,3 wt%) and RO water (16 wt%) at normal temperature to prepare blank pug, and putting the blank pug in a 55 ℃ incubator to be aged for 96 hours to obtain aged pug. And then extruding and molding the aged pug by using an extruder (the obtained blank is a fan-shaped blank with the cross section of 90 degrees), setting the heating temperature of the extruder to be 50 ℃ and the extrusion pressure to be 9.2Mpa. And (3) rapidly cooling the green body to 0 ℃ in 35s by adopting low-temperature nitrogen at the die opening of the honeycomb ceramic membrane die of the extruder, extruding the green body with a certain length, and cutting the green body to obtain the high-strength green body. And (3) freeze-drying the high-strength green body at-50 ℃ for 48h, and then sintering at 1750 ℃ for 3h to form the honeycomb ceramic membrane support. And finally, combining the four ceramic membrane components into a large-diameter combined honeycomb ceramic filter membrane product according to a set distance, wherein gaps between the adjacent ceramic membrane components are accumulated water flow channels. The bending degree of the product with the diameter of 120mm and the length of 1.2m prepared by the comparative example is less than 16mm, the deviation of the outer diameter is less than 23mm, and the yield is 37%.
Comparative example 4
Uniformly mixing aluminum oxide micro powder (35 mu m,73 wt%), silicon oxide micro powder (2um, 1.5 wt%), magnesium oxide (1 wt%), tung oil (0.5 wt%), gelatin powder (4 wt%), hydroxypropyl methyl cellulose (the gel temperature is 75 ℃,2 wt%) and RO water (18 wt%) at normal temperature to prepare blank pug, and putting the blank pug in a 55 ℃ heat preservation box for ageing for 96 hours to obtain the aged pug. And then extruding and molding the aged pug by using an extruder (the obtained blank is a fan-shaped blank with the cross section of 90 degrees), setting the heating temperature of the extruder to be 50 ℃ and the extrusion pressure to be 13.5Mpa. And (3) rapidly cooling the green body to 0 ℃ within 35 seconds by adopting low-temperature nitrogen at the die opening of the honeycomb ceramic membrane die of the extruder, extruding the green body with a certain length, and cutting the green body to obtain a high-strength green body. And (3) freeze-drying the high-strength green body at-50 ℃ for 48h, and then sintering at 1750 ℃ for 3h to form the honeycomb ceramic membrane support. And finally, combining the four ceramic membrane components into a large-diameter combined honeycomb ceramic filter membrane product according to a set distance, wherein a gap between every two adjacent ceramic membrane components is a ponding flow channel. The bending degree of the product with the diameter of 120mm and the length of 1.2m prepared by the comparative example is less than 11mm, the deviation of the outer diameter is less than 12mm, and the yield is 72 percent.
A comparison of the products obtained in the examples and comparative examples is shown in the following table:
(1) Deviation of outer diameter: the circular ceramic membrane blank body can collapse into an ellipse under the influence of gravity, and the difference value of the major diameter and the minor diameter of the ellipse is the outer diameter deviation.
(2) Curvature: the ceramic membrane blank can be bent and deformed in the preparation process under the influence of gravity, the ceramic membrane tube is placed on a plane, and the distance between the plane and the arched position with the maximum deformation is the bending degree of the ceramic membrane tube.
The above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (4)
1. A preparation method of a large-diameter combined honeycomb ceramic filter membrane is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparing blank body pug, and ageing for 72-96h at 50-55 ℃ to obtain aged pug, wherein the formula of the blank body pug is as follows: 72-74wt% of aluminum oxide micro powder, 1-2wt% of silicon oxide micro powder, 0.8-1.2wt% of magnesium oxide, 0.4-0.6wt% of tung oil, 2-4wt% of gelatin powder, 3-6wt% of hydroxypropyl methyl cellulose with the gel temperature of 40-100 ℃, and the balance of RO water; the grain diameter of the alumina micro powder is 30-40 μm, and the grain diameter of the silicon oxide micro powder is 1.5-2.5 μm;
(2) Extruding the stale pug into a sector blank with the cross section of 0-180 degrees by an extruder at the temperature of 40-100 ℃ and under the extrusion pressure of 5-7MPa, rapidly cooling the blank to 0-5 ℃ within 20-35s by using low-temperature nitrogen while extruding, and cutting after extruding to a set length to obtain a high-strength blank;
(3) Freeze-drying the high-strength green body at-52 to-48 ℃ for 45 to 50 hours, and sintering to obtain the honeycomb ceramic membrane support body, wherein the sintering temperature is 1745 to 1750 ℃ and the sintering time is 2.5 to 3.5 hours;
(4) Preparing at least one filter membrane layer on the honeycomb ceramic membrane support body to obtain a ceramic membrane component;
(5) And assembling at least two ceramic membrane components according to a set interval to form the large-diameter combined honeycomb ceramic filter membrane with a circular cross section, the diameter of 110-130mm and the length of 1.1-1.3m, wherein a gap between adjacent ceramic membrane components is a ponding flow channel.
2. The method of claim 1, wherein: the formula of the blank body pug in the step (1) is as follows: 73wt% of aluminum oxide micro powder, 1.5wt% of silicon oxide micro powder, 1wt% of magnesium oxide, 0.5wt% of tung oil, 2-4wt% of gelatin powder, 3-6wt% of hydroxypropyl methyl cellulose and the balance of RO water.
3. The method of claim 1, wherein: the particle size of the alumina micro powder is 35 mu m, and the particle size of the silica micro powder is 2 mu m.
4. The method of claim 1, wherein: the extrusion speed of the extruder in the step (2) is 0.01-0.012m/s.
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