CN107519764B - Method for producing an asymmetric tubular filter element blank and use thereof - Google Patents
Method for producing an asymmetric tubular filter element blank and use thereof Download PDFInfo
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- CN107519764B CN107519764B CN201710637642.6A CN201710637642A CN107519764B CN 107519764 B CN107519764 B CN 107519764B CN 201710637642 A CN201710637642 A CN 201710637642A CN 107519764 B CN107519764 B CN 107519764B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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
- B01D69/105—Support pretreatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/06—Tubular membrane modules
- B01D63/061—Manufacturing thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/06—Tubular membrane modules
- B01D63/062—Tubular membrane modules with membranes on a surface of a support tube
- B01D63/063—Tubular membrane modules with membranes on a surface of a support tube on the inner surface thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
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Abstract
The invention discloses a method for manufacturing an asymmetric tubular filter element blank, which comprises the following steps: 1) obtaining a support body and slurry: the slurry comprises a first raw material powder and a dispersant; the aperture of the support body is 1-3 times of the particle size of the first raw material powder; 2) grouting: standing the support body and blocking the lower part of the support body, then filling the inside of the support body with the slurry and keeping the inside for at least 10s, and then naturally flowing the slurry in the support body from the lower part; 3) preparing the coating: the support body is placed upside down, two ends of the support body are sealed, then the support body is rotated in the horizontal direction, so that the first raw material powder in the injected slurry in the support body is attached to the inner wall of the support body under the centrifugal action, and the dispersing agent in the injected slurry passes through the pipe wall of the support body under the centrifugal action, and therefore a precursor of the asymmetric tubular filter element blank is obtained; 4) and (5) drying.
Description
Technical Field
The invention relates to the technical field of asymmetric tubular filter elements, in particular to a manufacturing method and application of an asymmetric tubular filter element blank.
Background
The asymmetric tubular filter element refers to an asymmetric tubular filter element with the filter pore size changing in a gradient manner in the filter direction. The pore diameter of the asymmetric tubular filter element is sequentially increased or decreased from inside to outside along the radial direction. Wherein, the inner layer structure of the asymmetric tubular filter element with the sequentially increased pore diameter is called an inner membrane, and the outer layer structure is called a support body; the inner layer structure of the asymmetric tubular filter element with the sequentially reduced pore size is called a support body, and the outer layer structure is called an outer membrane; the inner and outer membranes may be collectively referred to as membrane layers.
For asymmetric tubular filter elements with a membrane layer produced by powder metallurgy, the following steps are generally included: 1) adhering slurry (prepared by adding membrane powder into a dispersing agent) on the surface of the support body and drying to form a coating; 2) and carrying out secondary sintering on the support body attached with the slurry to convert the coating into an inner film or an outer film (membrane layer). Currently, the main preparation process of the adhesive slurry is spraying or dipping.
Spraying is easy to understand, and although spraying is easy to form an inner film or an outer film independently, the spraying is difficult to form a coating with uniform thickness, so that the surface of the final film layer is uneven, cracks are easy to generate during sintering and filtering, or the pore diameter of the film layer is not uniform.
The impregnation requires a special equipment to prevent the slurry from being applied to the outside of the support when preparing the inner film or to the inside of the support when preparing the outer film. For example, the following methods are mainly used for preparing the inner film: preparing a certain volume of slurry, pouring the slurry into a tubular membrane dipping tool, hermetically dipping the outer surface of the support body into the slurry, and adsorbing a certain amount of slurry on the inner surface of the support body after a certain time. The membrane dipping process is complex in operation process, slurry attached to the surface of the support body flows downwards after dipping is finished, one flow mark is formed on the inner surface of the support body, the thickness of a membrane layer is uneven, cracks are generated during sintering, and the aperture of an inner membrane is uneven.
Disclosure of Invention
The invention mainly aims to provide a manufacturing method and manufacturing equipment of an asymmetric tubular filter element blank, so as to solve the problems of uneven film thickness and pore size distribution and cracks of an asymmetric tubular filter element in the prior art. Meanwhile, a manufacturing method and a manufacturing device of the asymmetric tubular filter element are also provided, so that the asymmetric tubular filter element with excellent performance is prepared.
To achieve the above objects, according to one aspect of the present invention, there is provided a method of manufacturing an asymmetric tubular filter element blank. The asymmetric tubular filter element blank comprises a tubular and porous support body and a coating layer positioned on the inner wall of the support body, wherein the coating layer is formed by attaching slurry to the inner wall of the support body and drying the slurry, and the manufacturing method of the asymmetric tubular filter element blank comprises the following steps:
1) obtaining a support body and slurry: the slurry comprises a first raw material powder and a dispersant; the aperture of the support body is 1-3 times of the particle size of the first raw material powder;
2) grouting: standing the support body and blocking the lower part of the support body, then filling the inside of the support body with the slurry and keeping the inside for at least 10s, and then naturally flowing the slurry in the support body from the lower part;
3) preparing the coating: the support body is placed upside down, two ends of the support body are sealed, then the support body is rotated in the horizontal direction, so that the first raw material powder in the injected slurry in the support body is attached to the inner wall of the support body under the centrifugal action, and the dispersing agent in the injected slurry passes through the pipe wall of the support body under the centrifugal action, and therefore a precursor of the asymmetric tubular filter element blank is obtained;
4) and (3) drying: and drying the precursor to obtain the asymmetric tubular filter element blank.
The 'standing' means that the central axis of the support body is vertical to the horizontal plane; the 'upside down' refers to that the central axis of the support body is parallel to the horizontal plane; the expression "rotating the support body in the horizontal direction" means that a rotation axis for rotating the support body is parallel to the central axis; the manufacturing method of the asymmetric tubular filter element blank according to the invention for the first time envisages the application of the centrifuge principle to the attachment of slurry, which may lead to the following advantages:
1) under the action of centrifugal force, the first raw material powder further moves towards the support body, so that the first raw material powder is in close contact with the support body, the bonding force between the sintered film layer and the support body can be improved, and the film layer is not easy to fall off; meanwhile, in the conventional preparation method, the asymmetric tubular filter element blank needs to be pressed after being dried to improve the compactness of the first raw material powder, and the first raw material powder in the asymmetric tubular filter element blank prepared by the preparation method of the application is accumulated more compactly, so that the pressing and filtering can be cancelled or the pressing time or the pressing force can be reduced;
2) the first raw material powder in the slurry is subjected to different centrifugal forces due to different sizes, the first raw material powder with larger particle size is subjected to a large centrifugal force and reaches the surface of the support body firstly, and the first raw material powder with smaller particle size is subjected to a small centrifugal force and then reaches the surface of the support body, so that the coating has a layered powder layer structure, each layer is provided with the first raw material powder with basically consistent particle size, and the membrane layer sintered by the coating has uniform pore diameter and smooth and flat surface;
3) the dispersing agent penetrates through the pipe wall of the support body under the action of centrifugal force and is thrown out, so that the drying time is reduced, the sintering time is shortened, the stress concentration generated by the first raw material powder during sintering is reduced, and cracks and pinholes are prevented from being generated on the film layer;
4) the slurry which is not firmly adhered to the support body also has certain fluidity, the support body rotates in the horizontal direction under the centrifugal action, so that the slurry is uniformly redistributed and firmly combined with the support body, and the obtained film layer has higher quality;
5) because the pore distribution of the support is tortuous, the first raw meal in the slurry is difficult to pass through the walls of the support so as to be thrown out; however, if the particle size of the first raw material powder is large, the first raw material powder is difficult to partially enter pores of the support, so that the bonding force between the film layer and the support is poor, and the film layer is easy to fall off; therefore, in order to further ensure that the first raw material powder is not thrown out and the bonding force between the film layer and the support is stronger, the pore diameter of the support is preferably 1 to 3 times the particle diameter of the first raw material powder; preferably, the pore diameter of the support is 1.8 to 2.5 times the particle diameter of the first raw material powder.
Further, the thickness of the pipe wall of the support body is 1-6 mm; the inner diameter of the support body is 20-100 mm; the thickness of the coating is 0.01-2 mm. Since the support body is subject to centrifugal action, the support body needs to have a certain thickness and inner diameter in order to prevent deformation of the support body, so as to obtain a suitable rigidity. And the aperture of the film layer is small, so that when the thickness of the coating is 0.01-2 mm, the film layer obtained by sintering can reduce the filtering pressure on the premise of keeping a good filtering effect. Preferably, the thickness of the pipe wall of the support body is 2-4 mm; the inner diameter of the support body is 30-75 mm; the thickness of the coating is 0.05-1 mm.
Further, the time for filling the inside of the support body with the slurry is 15 to 35 seconds. Thus, a coating of suitable thickness is obtained.
Furthermore, the rotating speed of the support body is 100-500 r/min, and the rotating time is 2-20 min. If the rotating speed is too slow, the efficiency is too low; if the rotation speed is too high, not only may the dispersing agent be rapidly thrown out and the first raw powder may not be distributed uniformly, but also there is a high demand for the rigidity of the support. Preferably, the rotating speed of the support body is 200-300 r/min, and the rotating time is 5-15 min.
Further, the preparation of the support comprises the following steps: 1) preparing a second raw material powder, and then pressing the second raw material powder into a support body precursor, wherein the support body precursor has the shape of the support body; 2) and sintering the support body precursor to obtain the support body. The support body and the film layer are both made of sintered metal porous materials or sintered ceramic porous materials, so that the support body can bear high temperature in the coating sintering process, and can form metallurgical bonding with the film layer in the coating sintering process, and the bonding force is stronger; and the precursor of the support body is directly pressed by second raw material powder, and the support body has better rigidity easily, and can reduce the thickness of the support body on the premise of bearing higher centrifugal force.
Further, the method adopts equipment comprising a film soaking component, a sealing part and a driving component for driving the supporting body to rotate in the horizontal direction; the membrane immersing component comprises a feeding device, a plug matched with the bottom of the support body when the support body is vertically placed, a liquid discharge pipe penetrating through the plug and a valve arranged on the liquid discharge pipe; the sealing part comprises a first sealing part and a second sealing part which are respectively matched with two ends of the supporting body; the driving assembly comprises a rotating shaft connected with the first sealing part and the second sealing part and a motor driving the rotating shaft to rotate. From this, this equipment structure is simple, collects slip casting and centrifugation as an organic whole, can show promotion production efficiency.
To achieve the above object, according to another aspect of the present invention, there is also provided a method of manufacturing an asymmetric tubular filter element. The method for preparing the asymmetric tubular filter element comprises the following steps:
1) preparing an asymmetric tubular filter element blank by adopting the manufacturing method of the asymmetric tubular filter element blank;
2) sintering the asymmetric tubular filter element blank to convert the coating in the asymmetric tubular filter element blank into a membrane layer with a filtering function, thus obtaining the asymmetric tubular filter element.
The asymmetric tubular filter element blank prepared by the manufacturing method of the asymmetric tubular filter element blank is sintered to obtain the asymmetric tubular filter element, the thickness and the pore size of a membrane layer are uniformly distributed, and cracks and pinholes are avoided. The membrane layer is an inner membrane.
Further, the support and the membrane layer are made of sintered metal porous materials or sintered ceramic porous materials having the same affinity. This ensures that the support and the film layer are not separated from each other due to the difference in material.
Further, the particle size of the first raw material powder is 1-12 μm; the second raw material powder has a particle size of-200 to +400 meshes. Thus, the pore diameter of the support body can be easily matched with the particle diameter of the first raw material powder, and an asymmetric tubular filter element with an appropriate pore diameter can be obtained.
In order to achieve the above object, according to another aspect of the present invention, there is also provided a manufacturing apparatus for an asymmetric tubular filter element blank, the asymmetric tubular filter element blank including a tubular and porous support body and a coating layer on an inner wall of the support body, the coating layer being formed by attaching a slurry to the inner wall of the support body and drying the slurry, the manufacturing apparatus including a membrane-immersing component, a sealing part, and a driving component for driving the support body to rotate in a horizontal direction; the membrane immersing component comprises a feeding device, a plug matched with the bottom of the support body when the support body is vertically placed, a liquid discharge pipe penetrating through the plug and a valve arranged on the liquid discharge pipe; the sealing part comprises a first sealing part and a second sealing part which are respectively matched with two ends of the supporting body; the driving assembly comprises a rotating shaft connected with the first sealing part and the second sealing part and a motor driving the rotating shaft to rotate.
During the use, at first adopt feed arrangement to make the supporter in be full of thick liquids, make partial thick liquids attach to the internal surface of supporter under self pressure effect, then the starter motor makes the pivot rotate, can make the supporter rotate to make thick liquids distribute evenly and increase the cohesion of first raw materials powder and supporter. Therefore, the manufacturing equipment of the asymmetric tubular filter element blank has a simple structure, can prepare the coating with uniform thickness, and can remarkably improve the production efficiency.
Further, the membrane immersing assembly further comprises a storage tank for containing the slurry, and the storage tank is communicated with the liquid discharge pipe; the feeding device comprises a liquid inlet pipe connected with the storage tank and a pump arranged on the liquid inlet pipe. Thereby, the slurry discharged from the drain pipe can be directly reused.
Further, a first controller that controls the valve to close and a second controller that controls the operation of the pump are included. Thereby, the thickness of the coating is intelligently controlled.
Further, a stirrer is arranged in the storage tank. Thereby, the components of the slurry in the storage tank are uniformly distributed all the time.
The grouting mechanism comprises a slurry flowing channel which is arranged on the first sealing part and/or the second sealing part and enables the inside and the outside of the support body to be communicated. Thus, when the amount of the slurry adhered by the membrane-immersed assembly is insufficient, the slurry can be increased by the grouting mechanism.
The relative position relationship between the grouting mechanism and the driving assembly can be three types:
first, the rotating shaft and the slurry flowing channel are not overlapped, that is, two holes need to be formed in the first sealing portion and/or the second sealing portion, at this time, the grouting mechanism should further include a first plug matched with the slurry flowing channel, and since the rotating shaft does not participate in grouting, the rotating shaft may be of a solid structure. This prevents the slurry from being thrown out of the slurry flow channel during centrifugation.
And secondly, the rotating shaft comprises a hollow tubular part which penetrates through the slurry flowing channel and is used for the slurry to flow, and the grouting mechanism further comprises a slurry outlet hole which is arranged on the hollow tubular part inside the supporting body and communicated with the inside of the supporting body and a grouting hole which is arranged on the hollow tubular part outside the supporting body. Thus, the paddle is distributed more evenly at the bottom of the support body before rotation, which is beneficial to obtain a coating with more even thickness.
And thirdly, the rotating shaft comprises a hollow tubular part which penetrates through the slurry circulation channel and is used for the slurry to flow, the grouting mechanism further comprises a slurry outlet hole which is arranged on the hollow tubular part inside the supporting body and is communicated with the inside of the supporting body, and a grouting hole which is arranged on the hollow tubular part outside the supporting body. Therefore, only one hole is formed in the sealing part, even if the rotating shaft and the slurry circulation channel are overlapped, the structure is more compact, and the sealing effect is better.
Further, the grouting device also comprises a second plug matched with the grouting hole. This prevents the slurry from being thrown out of the injection hole during centrifugation.
Furthermore, the first sealing part and/or the second sealing part are made of elastic materials; the plug is made of elastic materials. From this, easily acquire and sealed effectual.
Furthermore, the device also comprises a positioning mechanism for positioning the rotating shaft. Therefore, the rotation process of the support body is more stable.
Furthermore, the box body is further included, and a rotating hole matched with the rotating shaft is formed in the box body. Thus, the dispersant is recovered while preventing the dispersant from splashing.
Further, the thickness of the pipe wall of the support body is 1-6 mm; the inner diameter of the support body is 20-100 mm; the thickness of the coating is 0.01-2 mm. Since the support body is subject to centrifugal action, the support body needs to have a certain thickness and inner diameter in order to prevent deformation of the support body. And the aperture of the film layer is smaller, so that when the thickness of the coating is 0.01-2 mm, the film layer sintered by the coating can reduce the filtering pressure on the premise of keeping a better filtering effect. Preferably, the thickness of the pipe wall of the support body is 2-4 mm; the inner diameter of the support body is 30-75 mm; the thickness of the coating is 0.05-1 mm.
In order to achieve the above object, according to another aspect of the present invention, there is also provided an apparatus for manufacturing an asymmetric tubular filter element, which is sintered from an asymmetric tubular filter element blank, the manufacturing apparatus including an apparatus for manufacturing the asymmetric tubular filter element blank, an apparatus for drying the asymmetric tubular filter element blank, and an apparatus for sintering the asymmetric tubular filter element blank, wherein the apparatus for manufacturing the asymmetric tubular filter element blank is the above-mentioned apparatus for manufacturing the asymmetric tubular filter element blank.
The equipment for preparing the asymmetric tubular filter element has a simple structure, can prepare a film layer with uniform thickness and aperture and without defects of cracks, pinholes and the like, and can remarkably improve the production efficiency.
Therefore, the manufacturing method of the asymmetric tubular filter element blank introduces the centrifugal principle into the traditional coating preparation process, not only has simple process, but also can obtain the coating with very uniform thickness distribution. The manufacturing equipment of the asymmetric tubular filter element blank has a simple structure, and can obviously improve the preparation speed of the coating. The manufacturing method and the manufacturing equipment of the asymmetric tubular filter element applying the manufacturing method and the manufacturing equipment of the asymmetric tubular filter element blank can obviously improve the production efficiency of preparing the asymmetric tubular filter element and the quality of a membrane layer.
The invention is further described with reference to the following figures and detailed description. Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to assist in understanding the invention, and are included to explain the invention and their equivalents and not limit it unduly. In the drawings:
fig. 1 is a cross-sectional view of a membrane-impregnated assembly of an apparatus for manufacturing an asymmetric tubular filter element blank according to example 1 of the present invention.
Fig. 2 is a cross-sectional view of the seal and drive assembly of an apparatus for making an asymmetric tubular filter element blank according to example 1 of the present invention.
Fig. 3 is a cross-sectional view of the seal portion and drive assembly of the manufacturing apparatus of the asymmetric tubular filter element blank manufacturing apparatus of example 2 of the present invention.
Fig. 4 is a cross-sectional view of the seal and drive assembly of an apparatus for making an asymmetric tubular filter element blank according to example 3 of the present invention.
Fig. 5 is a cross-sectional view of the seal and drive assembly of an apparatus for making an asymmetric tubular filter element blank according to example 4 of the present invention.
Fig. 6 is a cross-sectional view of the seal and drive assembly of an apparatus for making an asymmetric tubular filter element blank according to example 5 of the present invention.
Fig. 7 is a cross-sectional view of the seal and drive assembly of an apparatus for making an asymmetric tubular filter element blank according to example 6 of the present invention.
The relevant references in the above figures are:
1: a support body;
21: a first seal portion;
22: a second seal portion;
3: a slurry flow channel;
4: a motor;
5: a rotating shaft;
51: a first rotating shaft;
52: a second rotating shaft;
53: a hollow tubular portion;
54: a cylindrical portion;
6: a first plug;
7: a slurry outlet;
8: grouting holes;
9: a second plug;
10: a positioning mechanism;
11: a plug;
12: a liquid discharge pipe;
13: a valve;
14: a storage tank;
15: a liquid inlet pipe;
16: a pump;
17: a stirrer.
Detailed Description
The invention will be described more fully hereinafter with reference to the accompanying drawings. Those skilled in the art will be able to implement the invention based on these teachings. Before the present invention is described in detail with reference to the accompanying drawings, it is to be noted that:
the technical solutions and features provided in the present invention in the respective sections including the following description may be combined with each other without conflict.
Moreover, the embodiments of the present invention described in the following description are generally only examples of a part of the present invention, and not all examples. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
With respect to terms and units in the present invention. The terms "comprising," "having," and any variations thereof in the description and claims of this invention and the related sections are intended to cover non-exclusive inclusions.
The asymmetric tubular filter element blank in the following specific embodiment of the present invention comprises a tubular and porous support body 1 and a coating layer on the inner wall of the support body 1, wherein the coating layer is formed by attaching slurry to the inner wall of the support body 1 and drying; the asymmetric tubular filter element is formed by sintering the asymmetric tubular filter element blank, and the coating is converted into a membrane layer with a filtering function in the sintering process. The term "air flux" refers to the amount of air permeated per kilopascal of filtration pressure per hour per square meter of filtration area.
Example 1
The manufacturing equipment of the asymmetric tubular filter element blank shown in fig. 1 and 2 comprises a membrane dipping assembly, a sealing part and a driving assembly for driving the supporting body 1 to rotate in the horizontal direction.
The membrane immersing component comprises a storage tank 14 for containing the slurry, a feeding device, a plug 11 matched with the bottom of the support body 1 when the support body is vertically placed, a liquid discharge pipe 12 penetrating through the plug 11 and a valve 13 arranged on the liquid discharge pipe 12.
The reservoir tank 14 is in communication with the drain pipe 12.
The feeding device comprises a liquid inlet pipe 15 connected with the storage tank 14 and a pump 16 arranged on the liquid inlet pipe 15.
The storage tank 14 is provided with a stirrer 17.
The sealing portion includes a first sealing portion 21 and a second sealing portion 22 respectively matched with both ends of the support body 1.
The first sealing portion 21, the second sealing portion 22 and the plug 11 are made of elastic materials, and the elastic materials are rubber.
The driving assembly comprises a rotating shaft 5 connected with the first sealing part 21 and the second sealing part 22 and a motor 4 driving the rotating shaft 5 to rotate.
And the device also comprises a positioning mechanism 10 for positioning the rotating shaft 5.
The box body is provided with a rotating hole matched with the rotating shaft 5.
Example 2
The manufacturing apparatus for the asymmetric tubular filter element blank of this example differs from the manufacturing apparatus for the asymmetric tubular filter element blank described in example 1 in that: as shown in fig. 3, the grouting device further includes a grouting mechanism, which includes a slurry flow channel 3 provided in the first sealing portion 21 and communicating the inside and the outside of the support body 1, and a first plug 6 matching with the slurry flow channel 3; the first plugs 6 are made of elastic materials, and the elastic materials are rubber.
Example 3
The manufacturing apparatus for the asymmetric tubular filter element blank of this example differs from the manufacturing apparatus for the asymmetric tubular filter element blank of example 2 in that: as shown in fig. 4, the second sealing portion 22 is also provided with the slurry flow passage 3 and the first plug 6.
Example 4
The manufacturing apparatus for the asymmetric tubular filter element blank of this example differs from the manufacturing apparatus for the asymmetric tubular filter element blank described in example 1 in that: as shown in fig. 5, the support body further comprises a grouting mechanism, wherein the grouting mechanism comprises a slurry flowing channel 3 which is arranged on the first sealing part 21 and the second sealing part 22 and is used for communicating the inside and the outside of the support body 1; the rotating shaft 5 comprises a hollow tubular part 53 which passes through the slurry flowing channel 3 and is used for the slurry to flow, the grouting mechanism also comprises a slurry outlet hole 7 which is arranged on the hollow tubular part 53 positioned in the supporting body 1 and is communicated with the inside of the supporting body 1, and a grouting hole 8 which is arranged on the hollow tubular part 53 positioned outside the supporting body 1; the grouting mechanism further comprises a second plug 9 matched with the grouting hole 8, and the second plug 9 is in threaded connection with the grouting hole 8.
Example 5
The manufacturing apparatus for the asymmetric tubular filter element blank of this example differs from the manufacturing apparatus for the asymmetric tubular filter element blank described in example 1 in that: as shown in fig. 6, the present invention further comprises a grouting mechanism including a slurry passage 3 provided in the second sealing portion 22 to communicate the inside and outside of the support body 1; the rotating shaft 5 comprises a first rotating shaft 51 connected with the first sealing part 21 and a second rotating shaft 52 connected with the second sealing part 22, the second rotating shaft 52 comprises a cylindrical part 54, the cylindrical part 54 is matched with the slurry circulation channel 3, and the grouting mechanism further comprises a grouting hole 8 arranged on the cylindrical part 54; the grouting mechanism further comprises a second plug 9 matched with the grouting hole 8, and the second plug 9 is in threaded connection with the grouting hole 8.
Example 6
The manufacturing apparatus for the asymmetric tubular filter element blank of this example differs from the manufacturing apparatus for the asymmetric tubular filter element blank of example 5 in that: as shown in fig. 7, the first seal portion 21 is also provided with the slurry flow passage 3, and correspondingly, the first shaft 51 includes a cylindrical portion 54, the cylindrical portion 54 is engaged with the slurry flow passage 3, and the grouting mechanism further includes a grouting hole 8 provided in the cylindrical portion 54.
The manufacturing equipment of the asymmetric tubular filter element comprises manufacturing equipment of the asymmetric tubular filter element, drying equipment of the asymmetric tubular filter element blank and sintering equipment of the asymmetric tubular filter element blank in one of embodiments 1 to 6, wherein the equipment for drying the asymmetric tubular filter element blank and the equipment for sintering the asymmetric tubular filter element blank are both existing equipment.
In order to more clearly illustrate the beneficial effects of the manufacturing method of the asymmetric tubular filter element blank according to the present invention, specific examples 7 to 11 are described below, wherein the manufacturing apparatuses of the asymmetric tubular filter element blank according to example 1 are used in the examples 7 to 11.
The methods of examples 7-11 for making asymmetric tubular filter elements each include the steps of:
(1) preparation of the support 1:
adding titanium powder and aluminum powder serving as second raw material powder, wherein the titanium powder and the aluminum powder are-200 to +400 meshes in particle size, 66.7 parts in parts by weight and-200 to +400 meshes in particle size, and 33.3 parts in parts by weight into a V-shaped mixer, and mixing for 8 hours; the meaning of "-200- +400 mesh" is: the second raw material powder can leak through 200 meshes and can not leak through 400 meshes, when the second raw material powder with the mesh number is screened, a 400-mesh screen is placed under the 200-mesh screen, and first powder with-200 to +400 meshes is left on the 400-mesh screen;
selecting stearic acid as a granulating agent, adding the stearic acid into alcohol at 70 ℃ for dissolution, then adding the second raw material powder mixed in the step I into a mixing machine, slowly and uniformly adding a stearic acid solution in the stirring process, stirring for 5 hours, then granulating through a granulator, selecting a screen with 30 meshes, and then drying in an oven at 50 ℃;
assembling the mold, adding the granulated second raw material powder into the mold cavity, pressing the second raw material powder into a tubular support body precursor by a cold isostatic press, and demolding;
putting hollow spheres with the particle size of 30 meshes into a cavity of the support body precursor, putting the support body precursor into a sintering boat, putting the support body precursor into a furnace for sintering, wherein the sintering temperature is 1250 ℃, the sintering time is 6 hours, and cooling to obtain a support body 1, wherein the thickness, the inner diameter and the aperture of the support body 1 are shown in table 1;
(2) preparing slurry:
adding first raw material powder into a V-shaped mixer according to the requirements of particle size and type of the first raw material powder in the table 1, and mixing for 8 hours; wherein A is the aperture of the support body 1, B is the particle size of titanium powder in the first raw material powder, and C is the particle size of aluminum powder in the first raw material powder;
adding glycol into absolute ethyl alcohol, wherein the volume ratio of the glycol to the absolute ethyl alcohol is 1:9, and mixing uniformly;
slowly adding the mixed first raw material powder into the ethylene glycol-ethanol mixed solution in the stirring process, adding 2ml of ethylene glycol-absolute-ethanol mixed solution into every 1g of the first raw material powder, stirring for 30min, and then performing ultrasonic treatment for 10min to obtain slurry;
table 1 shows the composition and ratio of the first raw material powder.
(3) Preparing a coating:
installing the support body 1 prepared in the step (1) according to the connection relation shown in the figure 1, filling the inside of the support body 1 with the slurry and keeping the slurry for at least 10s, wherein the specific keeping time is shown in a table 2;
opening a valve 13, discharging the slurry inside the support body 1, and then installing the support body according to the connection relation shown in the figure 2;
starting the motor 4 to rotate the support body 1 for 2-20 min at the rotating speed of 100-500 r/min, wherein specific rotating parameters are shown in a table 2;
fourthly, natural drying is carried out for 1 hour, and an asymmetric tubular filter element blank is obtained;
table 2 shows the process parameters for the preparation of the coatings and the parameters of the coatings.
(4) And (3) sintering: and (3) putting hollow spheres with the particle size of 50 meshes into the cavity of the support body 1 with the coating prepared in the step (3), sintering according to the sintering parameters in the table 3, wherein the temperature rise speed in the whole sintering process is 3 ℃/min, and obtaining the asymmetric tubular filter element after sintering, wherein the pore diameter and the performance parameters of the asymmetric tubular filter element are shown in the table 3.
Table 3 shows the sintering process parameters of the coating and the parameters of the film layer.
The following conclusions can be drawn from examples 7 to 11:
1) when the aperture of the support body 1 is 1-3 times of the particle size of the first raw material powder, the first raw material powder can be prevented from being thrown out, and the bonding force between the film layer and the support body 1 is stronger; preferably, the pore diameter of the support body 1 is 1.8 to 2.5 times of the particle diameter of the first raw material powder;
2) the thickness of the pipe wall of the support body 1 is 1-6 mm; when the internal diameter of supporter 1 was 20 ~ 100mm, supporter 1 was not deformable in the rotation process, at this moment, the thickness of coating is 0.01 ~ 2mm, can reduce filtration pressure under the prerequisite that keeps better filter effect. Preferably, the thickness of the pipe wall of the support body 1 is 2-4 mm; the inner diameter of the support body 1 is 30-75 mm; the thickness of the coating is 0.05-1 mm;
3) when the rotating speed of the support body 1 is 100-500 r/min and the rotating time is 2-20 min, the high production efficiency can be kept, and the first raw material powder can be uniformly distributed; preferably, the rotating speed of the support body 1 is 200-300 r/min, and the rotating time is 5-15 min;
4) when the particle size of the first raw material powder is 1-12 mu m and the particle size of the second raw material powder is-200 to +400 meshes, the asymmetric tubular filter element with proper pore size and high air flux is easy to obtain;
5) the coating is obtained when the inside of the support 1 is filled with the slurry and kept for at least 10 s. When the time for filling the inside of the support body 1 with the slurry is 15 to 35 seconds, a coating having an appropriate thickness can be obtained.
Example 12
Example 12 differs from example 9 in that: the manufacturing equipment of the asymmetric tubular filter element blank of example 5 was used, that is, in the process of preparing the coating, after opening the valve 13 to discharge the slurry inside the support body 1, the support body 1 was installed in the connection relationship shown in fig. 6, then 50 ml of slurry was injected into the support body from the injection hole 8, then the second plug 9 was installed and the motor 4 was started. The thickness of the resulting coating was 0.75 mm.
The contents of the present invention have been explained above. Those skilled in the art will be able to implement the invention based on these teachings. All other embodiments, which can be derived by a person skilled in the art from the above description without inventive step, shall fall within the scope of protection of the present invention.
Claims (10)
1. A method of making an asymmetric tubular filter element blank comprising a tubular and porous support and a coating on an inner wall of the support, the coating being formed by attaching a slurry to the inner wall of the support and drying the slurry, the method comprising the steps of:
1) obtaining a support body and slurry: the slurry comprises a first raw material powder and a dispersant; the aperture of the support body is 1-3 times of the particle size of the first raw material powder;
2) grouting: standing the support body and blocking the lower part of the support body, then filling the inside of the support body with the slurry and keeping the inside for at least 10s, and then naturally flowing the slurry in the support body from the lower part;
3) preparing the coating: the support body is placed upside down, two ends of the support body are sealed, then the support body is rotated in the horizontal direction, so that the first raw material powder in the injected slurry in the support body is attached to the inner wall of the support body under the centrifugal action, and the dispersing agent in the injected slurry passes through the pipe wall of the support body under the centrifugal action, and therefore a precursor of the asymmetric tubular filter element blank is obtained;
4) and (3) drying: drying the precursor to obtain the asymmetric tubular filter element blank;
the support body is a rigid support body, the outer wall of the support body does not need to be supported and coated during centrifugation, and the two ends of the support body are directly connected with the rotating shaft after being sealed;
the device adopted by the method comprises a film soaking component, a sealing part and a driving component for driving the supporting body to rotate in the horizontal direction;
the membrane immersing component comprises a storage tank, a feeding device, a plug matched with the bottom of the support body when the support body is vertically placed, and a liquid discharge pipe penetrating through the plug; the slurry in the storage tank flows into the support body from the liquid inlet pipe, and the slurry in the support body flows into the storage tank from the liquid outlet pipe;
the sealing part comprises a first sealing part and a second sealing part which are respectively matched with two ends of the supporting body;
the driving assembly comprises a rotating shaft connected with the first sealing part and the second sealing part and a motor driving the rotating shaft to rotate.
2. A method of making an asymmetric tubular filter element blank as recited in claim 1, wherein: the aperture of the support body is 1.8-2.5 times of the particle size of the first raw material powder.
3. A method of making an asymmetric tubular filter element blank as recited in claim 1, wherein: the thickness of the pipe wall of the support body is 1-6 mm; the inner diameter of the support body is 20-100 mm; the thickness of the coating is 0.01-2 mm.
4. A method of making an asymmetric tubular filter element blank as recited in claim 3, wherein: and the time for filling the inside of the support body with the slurry is 15-35 s.
5. A method of making an asymmetric tubular filter element blank as recited in claim 1, wherein: the rotating speed of the support body is 100-500 r/min, and the rotating time is 2-20 min.
6. A method of making an asymmetric tubular filter element blank as recited in claim 1, wherein: the preparation of the support body comprises the following steps:
1) preparing a second raw material powder, and then pressing the second raw material powder into a support body precursor, wherein the support body precursor has the shape of the support body;
2) and sintering the support body precursor to obtain the support body.
7. A method of making an asymmetric tubular filter element blank as recited in claim 1, wherein: the membrane dipping assembly further comprises a valve arranged on the liquid discharge pipe.
8. A method of making an asymmetric tubular filter element comprising the steps of:
1) preparing an asymmetric tubular filter element blank by using the manufacturing method of the asymmetric tubular filter element blank according to any one of claims 1 to 7;
2) sintering the asymmetric tubular filter element blank to convert the coating in the asymmetric tubular filter element blank into a membrane layer with a filtering function, thus obtaining the asymmetric tubular filter element.
9. A method of making an asymmetric tubular filter element as in claim 8, wherein: the support body and the membrane layer are made of sintered metal porous materials or sintered ceramic porous materials with the same affinity.
10. A method of making an asymmetric tubular filter element as in claim 8, wherein: the particle size of the first raw material powder is 1-12 mu m.
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| FR2614808A1 (en) * | 1987-05-06 | 1988-11-10 | Castelletto Jean Paul | Method for producing thin layers of uniform thickness by coating a support and equipment for implementing this method |
| CN1708348A (en) * | 2002-10-25 | 2005-12-14 | 高技术与膜工业公司 | Membrane for tangential filtration and production method thereof |
| CN1947861A (en) * | 2006-11-03 | 2007-04-18 | 西北有色金属研究院 | Micro-porous metal film prepn. method |
| CN101323528A (en) * | 2008-07-15 | 2008-12-17 | 南京工业大学 | Preparation method of gradient ceramic tube with continuous holes |
| CN104307258A (en) * | 2014-09-30 | 2015-01-28 | 成都易态科技有限公司 | Asymmetric sintered inorganic porous filtering element and preparation process thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| FR2614808A1 (en) * | 1987-05-06 | 1988-11-10 | Castelletto Jean Paul | Method for producing thin layers of uniform thickness by coating a support and equipment for implementing this method |
| CN1708348A (en) * | 2002-10-25 | 2005-12-14 | 高技术与膜工业公司 | Membrane for tangential filtration and production method thereof |
| CN1947861A (en) * | 2006-11-03 | 2007-04-18 | 西北有色金属研究院 | Micro-porous metal film prepn. method |
| CN101323528A (en) * | 2008-07-15 | 2008-12-17 | 南京工业大学 | Preparation method of gradient ceramic tube with continuous holes |
| CN104307258A (en) * | 2014-09-30 | 2015-01-28 | 成都易态科技有限公司 | Asymmetric sintered inorganic porous filtering element and preparation process thereof |
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