CN114452829B - Disc type ceramic membrane and distribution method thereof - Google Patents

Disc type ceramic membrane and distribution method thereof Download PDF

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Publication number
CN114452829B
CN114452829B CN202210059054.XA CN202210059054A CN114452829B CN 114452829 B CN114452829 B CN 114452829B CN 202210059054 A CN202210059054 A CN 202210059054A CN 114452829 B CN114452829 B CN 114452829B
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ceramic membrane
supporting layer
support body
distribution method
support
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CN114452829A (en
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郝恩奇
何世斌
常启兵
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Chongqing Wudun Nano Technology Co ltd
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Chongqing Wudun Nano Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039Inorganic membrane manufacture
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039Inorganic membrane manufacture
    • B01D67/0041Inorganic membrane manufacture by agglomeration of particles in the dry state
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/10Supported membranes; Membrane supports
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02Inorganic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02Inorganic material
    • B01D71/024Oxides
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02Inorganic material
    • B01D71/024Oxides
    • B01D71/025Aluminium oxide

Abstract

The application belongs to the technical field of ceramic membranes, in particular to a disc-type ceramic membrane and a distribution method thereof, which specifically comprise the following steps: step one: paving a ceramic membrane support body raw material on a die to form a first support layer; step two: paving a loose body on the first supporting layer, wherein the loose body comprises combustible matters; step three: paving the ceramic membrane support body raw materials on the first support layer and the loose body to form a second support layer; step four: and (5) carrying out dry pressing, and then carrying out drying and calcining to form a ceramic membrane support finished product. The application adopts a support body integrated material distribution mode, reduces the deformation of the ceramic membrane, and ensures that the ceramic membrane has better filtering effect; the support body is integrated, so that the integral structure of the ceramic membrane is firmer, and the service life of the ceramic membrane is prolonged; the water collecting channel is formed on the support body by adopting the primary loose body cloth, so that the cloth working procedure is reduced, the accuracy of the cloth is improved, and the quality of the ceramic film is improved.

Description

Disc type ceramic membrane and distribution method thereof
Technical Field
The application belongs to the technical field of ceramic membranes, and particularly relates to a disc-type ceramic membrane and a distribution method thereof.
Background
Ceramic membranes (also known as inorganic ceramic membranes) are asymmetric membranes formed from inorganic ceramic materials prepared by a particular process. The ceramic membranes are divided into two types of tubular ceramic membranes and planar ceramic membranes. Micropores are densely distributed on the wall of the tubular ceramic membrane, raw material liquid flows in the membrane tube or outside the membrane under the action of pressure, micromolecular substances (or liquid) permeate the membrane, and macromolecular substances (or solid) are intercepted by the membrane, so that the purposes of separation, concentration, purification, environmental protection and the like are achieved. The plate ceramic membrane has dense micropores, and the permeation rate is different according to different molecular diameters of permeated substances within a certain pore diameter range of the membrane, the pressure difference at two sides of the membrane is used as driving force, the membrane is used as a filter medium, and under the action of certain pressure, when feed liquid flows through the surface of the membrane, only water, inorganic salt and micromolecular substances are allowed to permeate the membrane, and the suspended matters, glue, microorganisms and other macromolecular substances in the water are prevented from passing through. The ceramic membrane has the advantages of high separation efficiency, stable effect, good chemical stability, acid and alkali resistance, organic solvent resistance, bacteria resistance, high temperature resistance, pollution resistance, high mechanical strength, good regeneration performance, simple separation process, low energy consumption, simple and convenient operation and maintenance, long service life and the like, has been successfully applied to various fields of food, beverage, plant (medicine) deep processing, biological medicine, fermentation, fine chemical engineering and the like, and can be used for separation, clarification, purification, concentration, sterilization, desalination and the like in the technical process. The disc-type ceramic membrane has the outer shape of a flying disc, the inside of the disc-type ceramic membrane contains a spiral permeation channel, and a membrane layer with a separation function is arranged on the outer surface of the disc-type ceramic membrane.
The existing disc-type ceramic membrane is generally characterized in that a support body is firstly manufactured, a filtering membrane is coated on the upper surface and the lower surface of the support body, the process is complex, raw materials are firstly pressed to manufacture the support body in the preparation process, a water collecting channel is further required to be arranged on the support body, the support body is required to be pressed again when the filtering membrane is coated, the ceramic membrane is required to be pressed for multiple times in the preparation process of the ceramic membrane, the ceramic membrane is deformed in the pressing process, multiple times of shaping is required, the production efficiency is low, the position of the support body is changed due to the multiple times of shaping, and the filtering effect of the ceramic membrane is affected.
Disclosure of Invention
The scheme provides the disc-type ceramic membrane with high production efficiency and the material distribution method thereof.
In order to achieve the above purpose, the present solution provides a disc ceramic membrane distribution method, which specifically includes the following steps:
step one: selecting an intermediate product in which a ceramic membrane support body raw material is paved on a die to form a first support layer;
step two: paving a loose body on the first supporting layer, and forming a structure with mutual attraction acting force between the loose body and the first supporting layer, wherein the loose body comprises combustible materials;
step three: paving the ceramic membrane support body raw materials on the first support layer and the loose body to form a second support layer;
step four: and (5) carrying out dry pressing, and then carrying out drying and calcining to form a ceramic membrane support finished product.
Further, the ceramic membrane support material is in a slurry or dry powder form. Ceramic membranes can be made using a variety of morphologic materials.
Further, the material distributing device of the ceramic membrane support body can load charges which are the same as the electrical property of the raw materials of the dry powder ceramic membrane support body when distributing materials. The raw materials are better distributed on the die through the repulsion of the like charges, and meanwhile, the raw materials can be reduced from being separated from the die and dispersed everywhere.
In the first step, a bottom layer of the first supporting layer is paved on the die, and dry pressing is carried out. The bottom layer of the first supporting layer is formed on the die, and dry pressing can reduce gas in the first supporting layer during one-step forming, so that the pore size of the first supporting layer can be controlled more easily.
Further, the loose bodies are embedded on the surface of the first supporting layer by means of gravity acceleration or wind power or carry opposite electric charges between the loose bodies and the first supporting layer.
Further, in the third step, the loose body is parabolic, linear, folded line, spot-shaped, honeycomb-shaped or irregular. The loose bodies with specific shapes are selected according to specific requirements, so that water collecting channels with different shapes can be conveniently formed.
Further, the whole cloth diameter of the loose body is smaller than the first supporting layer diameter and the second supporting layer diameter.
Further, the impact force of the flow velocity of the second supporting layer on the loose body during laying is smaller than the mutual attraction acting force of the loose body and the first supporting layer.
And in the fourth step, the semi-finished ceramic membrane support is dried for 80-300 min at the temperature of 60-200 ℃ and then calcined at the temperature of 1250-1750 ℃.
In order to achieve the above purpose, the present solution provides a disc-type ceramic membrane, which is manufactured by the above-mentioned disc-type ceramic membrane distribution method.
The application adopts a support body integrated material distribution mode, reduces the deformation of the ceramic membrane, and ensures that the ceramic membrane has better filtering effect; the support body is integrated, so that the integral structure of the ceramic membrane is firmer, and the service life of the ceramic membrane is prolonged; the water collecting channel is formed on the support body by adopting the primary loose body cloth, so that the cloth working procedure is reduced, the accuracy of the cloth is improved, and the quality of the ceramic film is improved.
Drawings
Fig. 1 is a schematic structural diagram of embodiment 1 of the present application.
Fig. 2 is a schematic structural view of a support body according to embodiment 1 of the present application.
FIG. 3 is a physical diagram of a disc-type ceramic membrane according to example 1 of the present application.
Detailed Description
The following is a further detailed description of the embodiments:
reference numerals in the drawings of the specification include: the water collecting device comprises a top film 1, a bottom film 2, a water collecting through hole 3, a supporting body 4 and a water collecting channel 5.
Example 1:
a disc-type ceramic membrane, as shown in fig. 1, fig. 2 and fig. 3, specifically comprising: the separation filter layer comprises a top film 1 and a bottom film 2, wherein the top film 1 and the bottom film 2 are respectively positioned on the upper surface and the lower surface of the support body 4. The support body 4, the top film 1 and the bottom film 2 are integrally arranged; the support body 4 is in a flying saucer shape, and the center of the support body 4 is provided with a water collecting through hole 3. The peripheral end of the supporting body 4 is closed; the support body 4 is internally provided with a water collecting channel 5, the water collecting channel 5 is used for discharging filtered solution, and the water collecting channel 5 is communicated with the water collecting through hole 3.
The solution is permeated from the top film 1 of the separation filter layer, and under the action of the top film 1 or the bottom film 2, the pollutants are left on the top film 1 or the bottom film 2, and the filtered solution enters the water collecting channel 5 and finally enters the water collecting through hole 3. The integrated dry pressing forming technology of the support body 4 is adopted, the overall structure of the disc-type ceramic membrane support body 4 is firmer, and the service life of the ceramic membrane is prolonged; the deformation of the ceramic membrane is reduced integrally, the sintering speed is high, and the ceramic membrane has better filtering effect and lower cost.
The scheme also provides a distribution method of the disc-type ceramic membrane, which specifically comprises the following steps:
step one: the ceramic membrane support body 4 is prepared by arranging raw materials in a mould to form a first support layer, and the thickness of the first support layer after compaction is generally controlled to be 0.3-4 mm; the ceramic membrane support 4 is slurry or dry powder. Ceramic membranes can be made using a variety of morphologic materials. Before the slurry raw material is used, the raw material needs to be subjected to vacuum defoaming treatment for 45min, and redundant bubbles are removed. The ceramic membrane support 4 is made of ceramic powder, and the average diameter of the ceramic powder is 0.1-1 mu m. The ceramic powder is alumina, titania, cordierite, zirconia, bauxite or other material. The material distributing device of the ceramic membrane support 4 is charged with the same electric charge as the raw material of the dry powder ceramic membrane support 4 during material distribution. The raw materials are better distributed on the die through the repulsion of the like charges, and meanwhile, the raw materials can be reduced from being separated from the die and dispersed everywhere. Specifically, the capacitor plate and the electrode plate can be adopted to charge the raw materials of the dry powder ceramic membrane support body 4, the ion blower can also be adopted to charge the raw materials of the dry powder ceramic membrane support body 4, the temperature of the ion blower when the ion blower is adopted is 15-42 ℃, the higher the temperature is, the faster the polymer diffusion is, and the raw materials of the dry powder ceramic membrane support body 4 can be charged fully at the temperature.
When the first supporting layer is paved, a bottom layer of the first supporting layer is paved on the die, and dry pressing is carried out. The bottom layer of the first supporting layer is formed on the die, and dry pressing can reduce gas in the first supporting layer during one-step forming, so that the pore size of the first supporting layer can be controlled more easily. Specifically, the dry powder ceramic membrane support 4 raw materials in a plurality of dies can be simultaneously subjected to dry pressing under the pressure of 20-200 mpa for 20-30 min, so that the preparation efficiency of the ceramic membrane is improved.
Step two: paving a loose body on the first supporting layer, wherein the loose body comprises combustible matters; the height of the loose body is 0.1-4 mm. According to the designed internal structure of the disc-type membrane, the combustible material or the mixture of the combustible material and the raw material of the support body 4 is distributed, the shape of the combustible material can be straight lines, fold lines, parabolas, spots, hexagons, honeycombs, irregular lines and the like, the water flow channel of the disc-type membrane is formed after the part is burnt, and the thickness of the compacted flow channel layer is generally controlled to be 0.1-4 mm; the combustible material cloth adopts a mode of one-time whole cloth or sequentially carrying out cloth, the cloth efficiency can be increased by adopting one-time whole cloth, the manufacturing time of the ceramic membrane is shortened, the combustible material cloth of each part is more accurate by adopting a mode of sequentially distributing, and the cloth is convenient to form a required water collecting channel 5.
The combustible material is specifically carbon material or starch, and the starch and the carbon material are conveniently burned to form the water collecting channel 5. The structure that has the interattraction effort is formed between loose body and the first supporting layer, and loose body relies on gravity acceleration or wind-force embedding to carry the opposite electric charge of electric property between first supporting layer surface or the loose body and the first supporting layer, the velocity of flow of second supporting layer when laying is less than loose body and first supporting layer interattraction effort to the impact force of loose body. It is possible to prevent the loose body from being displaced during the distribution of the second support layer, affecting the formation of the water collecting channel 5.
Step three: paving the raw materials of the ceramic membrane support body 4 on the first support layer and the loose body to form a second support layer, compacting the second support layer, and controlling the thickness of the compacted second support layer to be 0.3-4 mm, wherein the thickness of the second support layer is the same as or close to that of the first support layer; the thickness of the first supporting layer is larger than that of the second supporting layer, and the thickness difference between the thickness of the first supporting layer and that of the second supporting layer ranges from 0mm to 0.2mm. The diameter of the whole cloth of the loose body is smaller than the diameters of the first supporting layer and the second supporting layer.
Step four: dry pressing and demoulding, and then drying and calcining to form a ceramic membrane support 4 finished product; dry pressing from the second supporting layer to the first supporting layer. The dry pressing is carried out by adopting a press, wherein the press is a press, a hydraulic press and an oil press for short, and the press refers to a forming machine for forming industrial products through pressure, and a hydraulic oil cylinder is generally adopted, so that the press is also called an oil press. The pressure of the dry pressure is 20-200 Mpa. The ceramic membrane has better green body strength and high compactness under the pressure and is easier to burn. In the step, the semi-finished product of the ceramic membrane support body 4 is dried for 80-300 min at the temperature of 60-200 ℃ and then calcined at the temperature of 1250-1750 ℃.
The water collecting through holes 3 of the ceramic membrane are distributed in the distribution stage, the concrete form of the water collecting channels 5 is the same, the distribution is dry pressed, and finally the water collecting through holes 3 are formed in a calcining mode. The ceramic membrane may be calcined and formed and then perforated to form the water collecting through hole 3.
The application adopts the integrated material distribution mode of the support body 4 to reduce the deformation of the ceramic membrane, so that the filtering effect of the ceramic membrane is better; the support body 4 is adopted to integrate the ceramic membrane, so that the integral structure of the ceramic membrane is firmer, and the service life of the ceramic membrane is prolonged; the water collecting channel 5 is formed on the support body 4 by adopting one-time loose body cloth, so that the cloth working procedure is reduced, the accuracy of cloth is improved, and the quality of a ceramic film is improved.
Example 2:
the embodiment is different from embodiment 1 in that in step four, firstly, the ceramic film semi-finished product is calcined for 1-2 hours at 1250-1300 ℃ and simultaneously is dispersed by ultrasonic wave; and heating for 30min to raise the calcining temperature to 1300-1750 ℃ for calcining and molding.
When the temperature is 1250-1300 ℃, the combustible material burns, oxygen in a space formed by the first supporting layer and the second supporting layer is consumed, a channel for circulating the space formed by the first supporting layer and the second supporting layer with outside air is smaller, the oxygen in the space formed by the first supporting layer and the second supporting layer is smaller, and when the temperature is 1250-1300 ℃, the combustible material burns to mainly generate CO gas, and the generated CO gas escapes to the outside through the first supporting layer and the second supporting layer to form CO at high temperature 2 The porosity, membrane flux and filtration efficiency of the support body 4 can be improved under the action of CO gas, so that the ceramic membrane has better separation performance, and bacteria and heavy metals can be adsorbed in the pore structure of the support body 4 especially in the process of medical wastewater and heavy metals. In the process, the combustible substances are fully contacted with oxygen by ultrasonic dispersion to form more CO gas, so that the porosity, membrane flux and filtration efficiency of the support body 4 are improved, and the sewage filtration efficiency of the top membrane 1 and the bottom membrane 2 is conveniently improved.
The temperature is increased for a period of time, the temperature is stabilized by 30min, the calcining temperature is increased to 1300-1750 ℃, ultrasonic dispersion is stopped at the temperature, the combustible is prevented from being dispersed, the formation of the water collecting channel 5 is influenced, the oxygen content in a space formed by the first supporting layer and the second supporting layer is extremely low and approaches to an anaerobic environment, at the moment, C substances in the combustible can react with titanium oxide and zirconium oxide, a layer of titanium carbide and zirconium carbide can be generated on the surface of the pore structure of the supporting body 4, and the rigidity of the pore structure of the supporting body 4 is increased.
The foregoing is merely exemplary embodiments of the present application, and specific structures and features that are well known in the art are not described in detail herein. It should be noted that modifications and improvements can be made by those skilled in the art without departing from the structure of the present application, and these should also be considered as the scope of the present application, which does not affect the effect of the implementation of the present application and the utility of the patent. The protection scope of the present application is subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.

Claims (9)

1. The disc type ceramic membrane distribution method is characterized by comprising the following steps of:
step one: selecting an intermediate product in which a ceramic membrane support body raw material is paved on a die to form a first support layer;
step two: paving a loose body on the first supporting layer, and forming a structure with mutual attraction acting force between the loose body and the first supporting layer, wherein the loose body comprises combustible materials; the loose body and the first supporting layer carry opposite charges;
step three: paving the ceramic membrane support body raw materials on the first support layer and the loose body to form a second support layer;
step four: and (5) carrying out dry pressing, and then carrying out drying and calcining to form a ceramic membrane support finished product.
2. The disc ceramic membrane distribution method according to claim 1, characterized in that: the ceramic membrane support body raw material is in a slurry state or a dry powder state.
3. The disc ceramic membrane distribution method according to claim 2, characterized in that: the material distributing device of the ceramic membrane support body can load charges which are the same as the electrical property of the raw materials of the dry powder ceramic membrane support body when distributing materials.
4. The disc ceramic membrane distribution method according to claim 1, characterized in that: in the first step, a bottom layer of a first supporting layer is paved on a die and dry pressing is carried out.
5. The disc ceramic membrane distribution method according to claim 1, characterized in that: in the third step, the loose body is parabolic, linear, folded linear, spotted, honeycomb or irregular.
6. The disc ceramic membrane distribution method according to claim 1, characterized in that: the diameter of the whole cloth of the loose body is smaller than the diameters of the first supporting layer and the second supporting layer.
7. The disc ceramic membrane distribution method according to claim 1, characterized in that: the impact force of the flow velocity of the second supporting layer on the loose body during laying is smaller than the mutual attraction acting force of the loose body and the first supporting layer.
8. The disc ceramic membrane distribution method according to claim 1, characterized in that: and step four, drying the semi-finished ceramic membrane support body at 60-200 ℃ for 80-300 min, and calcining at 1250-1750 ℃.
9. Disc ceramic membrane, characterized in that it is produced by a method according to any one of claims 1-6.
CN202210059054.XA 2022-01-18 2022-01-18 Disc type ceramic membrane and distribution method thereof Active CN114452829B (en)

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