CN114769597A - Method and device for preparing outer wall film layer of metal powder porous matrix tube - Google Patents

Method and device for preparing outer wall film layer of metal powder porous matrix tube Download PDF

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Publication number
CN114769597A
CN114769597A CN202210720615.6A CN202210720615A CN114769597A CN 114769597 A CN114769597 A CN 114769597A CN 202210720615 A CN202210720615 A CN 202210720615A CN 114769597 A CN114769597 A CN 114769597A
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CN
China
Prior art keywords
metal powder
porous matrix
powder porous
wall
matrix tube
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CN202210720615.6A
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Chinese (zh)
Inventor
高东
李�荣
李永利
邓颖
刘静
刘丹阳
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Western Baode Technologies Co ltd
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Western Baode Technologies Co ltd
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Priority to CN202210720615.6A priority Critical patent/CN114769597A/en
Publication of CN114769597A publication Critical patent/CN114769597A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24After-treatment of workpieces or articles
    • B22F3/26Impregnating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2027Metallic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/11Making porous workpieces or articles
    • B22F3/1146After-treatment maintaining the porosity
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F5/00Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
    • B22F5/10Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
    • B22F5/106Tube or ring forms

Abstract

The invention discloses a preparation method and a device of an outer wall film layer of a metal powder porous matrix tube, wherein the preparation device of the outer wall film layer of the metal powder porous matrix tube comprises a control and power supply mechanism, a pressurization mechanism, a liquid supply mechanism and a film preparation mechanism; the preparation method of the metal powder porous matrix tube outer wall film layer comprises the following steps: step one, soaking a metal powder porous matrix tube in alcohol; step two, mounting a metal powder porous matrix tube; step three, preparing slurry; setting a pressure parameter, a rack rotation parameter and a stirring parameter; step five, starting grouting; step six, checking the impregnation condition of the film layer through pressure relief, and preparing a wet film on the outer wall of the metal powder porous matrix pipe; and step seven, drying and sintering the wet film on the outer wall of the metal powder porous matrix tube prepared in the step six to prepare the film layer on the outer wall of the metal powder porous matrix tube. The preparation method and the device of the outer wall film layer of the metal powder porous matrix tube can be used for producing the powder matrix tube composite film filter core with good film-substrate combination in batch.

Description

Preparation method and device of metal powder porous matrix tube outer wall film layer
Technical Field
The invention relates to the technical field of porous filter membrane production, in particular to a method and a device for preparing an outer wall membrane layer of a metal powder porous matrix tube.
Background
The porous film is prepared on the surface of the metal carrier to obtain the stainless steel filter element, the stainless steel filter element has the advantages of high temperature resistance, corrosion resistance, high weldability, good heat dissipation, strong interception performance and the like, and the stainless steel filter element serving as a functional material for separating two phases (gas and liquid, liquid and solid) is widely applied to industries such as petrochemical industry, coal chemical industry, industrial waste gas treatment and the like, and the working conditions are harsh in environment and have high requirements on filtering precision. The strength of the stainless steel filter element is greatly influenced by the combination condition of the film layer and the substrate, and the film layer is easy to fall off due to poor combination; the thickness uniformity, porosity and pore diameter uniformity of the membrane layer have great influence on the filtration precision; in industrial application, the stainless steel filter element is almost uninterruptedly used in production for a long time, the filter element has a limit service life, needs to be replaced within a certain age, and the requirement on the filter element is high, so that the porous film preparation of the stainless steel filter element needs to be superior, and the production efficiency is high.
At present, the processes for preparing the porous film on the surface of the metal carrier comprise the following steps:
the spraying method comprises the following steps: the spraying process mainly comprises three parts of surface preparation, heating and spraying. Firstly, a clean substrate is placed in a special heating furnace, the heating temperature is usually 350-500 ℃, and then a special spray gun is used for spraying the sol to the surface of the hot substrate at a certain pressure and speed to form a gel film. The thickness of the film depends on the concentration of the sol, the pressure, the spray gun speed and the spray time. SnO2The preparation of electrothermal film is usually made by this method. The film prepared by the spraying method has poor thickness uniformity, poor wettability to a substrate and film-substrate bonding strength phaseThe pair is poor.
A pulling method: the whole clean substrate is immersed in the sol prepared in advance, and then the substrate is smoothly pulled out from the sol at a precisely controlled uniform speed, a uniform liquid film is formed on the surface of the substrate under the action of viscosity, gravity and surface tension, and then the solvent is rapidly evaporated, so that the sol attached to the surface of the substrate is rapidly gelled to form a gel film. The thickness of the film depends on the concentration, viscosity and pulling speed of the sol, the process parameter range is narrow, and the thickness consistency of the film is not high.
Casting: the casting film is adopted to form a film, the film with high aperture distribution and high film thickness consistency is obtained after stripping, and then the casting film is tightly combined with the matrix in a rolling mode. The tape casting method is suitable for preparing a film layer on the surface of a sheet silk screen matrix, and then the powder mesh composite membrane filter tube is obtained by tube rolling and welding, and cannot be used for a metal powder porous tube.
It is noted that this section is intended to provide a background or context to the embodiments of the disclosure that are recited in the claims. The description herein is not admitted to be prior art by inclusion in this section.
Disclosure of Invention
The embodiment of the invention provides a method and a device for preparing a film layer on the outer wall of a metal powder porous matrix tube, which are used for solving the problems of low filtration precision, uneven film layer thickness, low film-substrate bonding strength and the like in the prior art.
The embodiment of the invention provides a device for preparing a film layer on the outer wall of a metal powder porous matrix tube, which is characterized by comprising the following components: the control and power supply mechanism, the pressurization mechanism, the film preparation mechanism and the liquid supply mechanism;
the control and power supply mechanism consists of a control cabinet, a power supply, an electric wire, a motor, a pressure sensor, an air cylinder and a stirrer, wherein the control cabinet and the power supply are connected with the motor, the pressure sensor, the air cylinder and the stirrer through the electric wire;
the pressurizing mechanism consists of a compressed air tank, an air valve, a pressure gauge and an air pipe, wherein the air valve and the pressure gauge are arranged on the compressed air tank, and the air pipe is connected with the slurry pool and the compressed air tank through a joint;
the film making mechanism comprises a material rack and a mold, wherein the material rack is arranged in the mold, and a central shaft penetrates through the mold;
the liquid supply mechanism consists of a sealing cover, a slurry pool and a grouting pipe, slurry is arranged in the slurry pool, the sealing cover is arranged at the top of the slurry pool, a feeding port is arranged on one side of the slurry pool, the grouting pipe is arranged in the middle of the slurry pool, the grouting pipe is in butt joint with the grouting port, and the grouting pipe is connected with the grouting port through a sealing gasket.
In a preferred mode of the present invention, the stirrer is composed of a stirring motor, a stirring shaft and a stirring blade.
As a preferred mode of the invention, the central shaft is sequentially provided with a shaft sleeve I and a shaft sleeve II from inside to outside, the central shaft, the shaft sleeve I and the shaft sleeve II are connected through a shaft sleeve spacing device, the shaft sleeve II is provided with a bull gear and a bearing support rod, a bearing is arranged on the bearing support rod, a pinion is meshed with the bull gear, the bearing is connected with the pinion through a rolling shaft, a nut seat is arranged on the central shaft, a scraper plate is arranged on the nut seat and a support guide rail, and the rolling shaft is connected with a support shaft;
the material rest consists of a scraper, a supporting guide rail, a metal powder porous matrix tube and a supporting shaft, wherein two ends of the material rest are provided with a bearing and a bearing supporting rod, the bearing is arranged on the bearing supporting rod, the bearing supporting rod is arranged on the shaft sleeve I, and the metal powder porous matrix tube is connected with the supporting shaft through the bearing; the mold consists of an exhaust plug, a left mold, a right mold and a bottom mold, the bottom mold is provided with a grouting port, the left mold and the right mold are arranged on a guide table, the guide table is fixed on the bottom mold, and a limit boss is arranged in the middle of the guide table; grooves are carved at corresponding positions of the left die and the right die, sealing buckles are arranged on the left die and the right die, and vent plugs are arranged at the tops of the left die and the right die; the left die and the right die are opened, and the rolling shaft is connected with the supporting shaft.
In a preferred embodiment of the present invention, the bottom surface of the bottom mold is flush with the top end of the pouring pipe.
In a preferred embodiment of the present invention, the central shaft is a screw shaft at a middle portion thereof.
In a preferred embodiment of the present invention, the injection port is provided with a screen having a pore size of 50 μm.
As a preferred mode of the invention, 4-15 air exhaust plugs are respectively and uniformly distributed at the tops of the left die and the right die.
As a preferable mode of the invention, the distance between the bottom end of the grouting pipe and the bottom of the slurry pool is 50 mm.
The embodiment of the invention provides a preparation method of an outer wall film layer of a metal powder porous matrix tube, which comprises the following steps:
step one, soaking a metal powder porous matrix tube by alcohol;
secondly, plugging two ports of the metal powder porous matrix tube by using a conical plug head, installing and fixing the metal powder porous matrix tube on a supporting shaft, installing a filter screen, cleaning the inner surface of the die, and closing a left die and a right die; 3-8 metal powder porous matrix pipes are installed;
step three, preparing slurry, wherein the preparation ratio of the polyvinylpyrrolidone to the ethanol solution is 5% -10%; adding the powder into a polyvinylpyrrolidone ethanol solution according to the proportion of 850 g/L-1200 g/L, and injecting slurry into a slurry pool from a feed inlet;
setting pressure parameters, rack rotation parameters and stirring parameters;
step five, starting grouting, dipping the metal powder porous matrix tube under pressure, and enabling the material rest to rotate in the die at a constant speed;
step six, releasing pressure, enabling slurry to fall back, continuously rotating the material rest, opening the left die and the right die, checking the impregnation condition of the film layer, enabling the porous metal powder base pipe to rotate if the impregnation effect is good, and directly scraping and pressing the film layer by a scraper to prepare a wet film on the outer wall of the porous metal powder base pipe;
and step seven, drying and sintering the wet film on the outer wall of the metal powder porous matrix tube prepared in the step six to prepare the film layer on the outer wall of the metal powder porous matrix tube.
As a preferable mode of the present invention, the stirrer in the fourth step is started once every 30min, and is stirred for 2-5min once, and the stirring speed is 30 rad/min.
According to the preparation method and the device for the outer wall film layer of the metal powder porous matrix tube, the metal powder porous matrix tube is soaked in alcohol, so that the pore channel of the matrix tube is in a saturated state, and then, by virtue of a pressurizing and bottom grouting mechanism, fine powder suspended particles in feed liquid are strongly, densely and uniformly attached to the outer wall of the powder matrix tube without penetrating into the pore channel of the matrix tube, so that a hole sealing state is achieved, and the air permeability of the powder film tube is ensured while the filtering precision is improved; and scraping and pressing the film layer by using a scraper, and finally preparing the porous film with high filtration precision, uniform pore diameter, high air permeability, uniform film layer thickness and high film-substrate bonding strength on the outer wall of the metal powder porous matrix tube. Further, the powder matrix tube composite membrane filter element with higher consistency of membrane thickness and pore size distribution and good membrane-base combination can be produced in batches.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic diagram of an apparatus for preparing a membrane layer on the outer wall of a porous matrix tube made of metal powder according to an embodiment of the present invention;
FIG. 2 is a partial right side view of FIG. 1;
FIG. 3 is an enlarged view of a portion of FIG. 1;
FIG. 4 is a flow chart of a method for forming a membrane layer on the outer wall of a metal powder porous matrix tube according to an embodiment of the present invention;
FIG. 5 is a scanning electron microscope image of an outer wall film layer of a metal powder porous matrix tube according to an embodiment of the present invention.
In the figure: 1. compressed air tank, 2 air valve, 3 pressure gauge, 4 air pipe, 5 pressure sensor, 6 electric wire, 7 control cabinet and power supply, 8 motor, 9 central shaft, 10 shaft sleeve I, 11 shaft sleeve II, 12 shaft sleeve spacing device, 13 bearing, 14 bearing support rod, 15 rolling shaft, 16 pinion, 17 gear wheel, 18 scraper, 19 nut seat, 20 support guide rail, 21 metal powder porous base body pipe, 22. the concrete pouring device comprises a venting plug, a support shaft 23, a support column 24, a ground support column 25, an air cylinder 26, a left mold 27, a right mold 28, a sealing buckle 29, a sealing bearing 29, a bottom mold 30, a limiting boss 31, a guide table 32, a guide table 33, a grouting opening 34, a filter screen 35, a sealing gasket 36, a sealing cover 37, a feeding opening 38, a slurry pool 39, slurry 40, a stirrer 41 and a grouting pipe.
Detailed Description
In order to make those skilled in the art better understand the technical solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined or explained in subsequent figures.
The invention relates to a preparation device of an outer wall film layer of a metal powder porous matrix tube, which is characterized in that a sintered metal powder porous tube is used as a matrix, and a wet film of the outer wall of the metal powder porous matrix tube is prepared by the preparation device of the outer wall film layer of the metal powder porous matrix tube as shown in figure 1.
The average pore diameters of three common sintered metal powder porous matrix tubes are respectively 10-13 μm, 23-25 μm and 36-38 μm, and the outer walls of the three common sintered metal powder porous matrix tubes are coated with film layers with matched powder particle diameters, so that higher filtering precision can be achieved, and meanwhile, higher air permeability is still achieved.
The device for preparing the outer wall film layer of the metal powder porous matrix tube comprises a control and power supply mechanism, a pressurizing mechanism, a film preparation mechanism and a liquid supply mechanism, and is shown in figures 1-3.
The control and power supply mechanism consists of a control cabinet and power supply 7, an electric wire 6, a motor 8, a pressure sensor 5, a cylinder 25 and a stirrer 40, wherein the control cabinet and power supply 7 are connected with the motor 8, the pressure sensor 5, the cylinder 25 and the stirrer 40 through the electric wire 6, the motor 8 is connected with a central shaft 9, a shaft sleeve I10 and a shaft sleeve II 11 through the electric wire 6, the cylinder 25 is connected with a left die 26 and a right die 27, and the central shaft 9 is arranged on the ground through a ground pillar 24;
the motor 8 controls the transmission of the central shaft 9, the shaft sleeve I10 and the shaft sleeve II 11, the pressure sensor 5 monitors the air pressure in the slurry pool 38 in real time, the air cylinder 25 controls the opening and closing actions of the left die 26 and the right die 27, and the stirrer 40 consists of a stirring motor, a stirring shaft and stirring blades and has the functions of preventing slurry from settling and ensuring that the concentration of the slurry is constant all the time;
a bearing is fixed at the top end of the ground pillar 24;
the pressurizing mechanism consists of a compressed air tank 1, an air valve 2, a pressure gauge 3 and an air pipe 4, wherein the air valve 2 and the pressure gauge 3 are arranged on the compressed air tank 1, and the air pipe 4 is connected with the slurry tank 38 and the compressed air tank 1 through a joint;
the pneumatic feeding liquid level applies downward pressure to enable the slurry 39 to enter the mold from the bottom of the slurry pool 38 through the grouting pipe 41; the pressurization is divided into 4 stages: grouting and filling, boosting, maintaining pressure and relieving pressure, accurately controlling the grouting and film adsorption processes, and strongly attaching suspended particles in feed liquid to the outer wall of the metal powder porous matrix tube 21 under the action of pressure, wherein the suspended particles are distributed more densely and uniformly;
the film making mechanism comprises a material rack and a mold, wherein the material rack is arranged in the mold, and a central shaft 9 penetrates through the mold;
the central shaft 9 is sequentially provided with a shaft sleeve I10 and a shaft sleeve II 11 from inside to outside, the central shaft 9, the shaft sleeve I10 and the shaft sleeve II 11 are connected through a shaft sleeve spacing device 12, the shaft sleeve II 11 is provided with a large gear 17 and a bearing support rod 14, a bearing 13 is arranged on the bearing support rod 14, a small gear 16 is meshed with the large gear 17, the bearing 13 is connected with the small gear 16 through a rolling shaft 15, a nut seat 19 is arranged on the central shaft 9, and a scraper 18 is arranged on the nut seat 19 and a support guide rail 20;
the material rest consists of a scraper 18, a supporting guide rail 20, a metal powder porous matrix tube 21 and a supporting shaft 23, wherein a bearing 13 and a bearing supporting rod 14 are arranged at two ends of the material rest, the bearing 13 is arranged on the bearing supporting rod 14, the bearing supporting rod 14 is arranged on a shaft sleeve I10, and the metal powder porous matrix tube 21 is connected with the supporting shaft 23 through the bearing 13;
the mold consists of an exhaust plug 22, a left mold 26, a right mold 27 and a bottom mold 30, the bottom mold 30 is provided with a grouting port 33, the left mold 26 and the right mold 27 are arranged on a guide table 32, the guide table 32 is fixed on the bottom mold 30, a limiting boss 31 is arranged in the middle of the guide table 32, grooves are carved in corresponding positions of the left mold 26 and the right mold 27, sealing buckles 28 are arranged on the left mold 26 and the right mold 27, and the exhaust plug 22 is arranged at the top of the left mold 26 and the right mold 27; the left die 26 and the right die 27 are opened, and the rolling shaft 15 is fixedly connected with the supporting shaft 23;
the bottom surface of the bottom die 30 is flush with the top end of the grouting pipe 41;
the bottom of the mould is connected with a slurry pool 38 through a grouting port 33;
the middle part of the central shaft 9 is provided with a lead screw which is used for the linear reciprocating motion of a nut seat 19;
the grouting port 33 is provided with a filter screen 34, and the aperture of the filter screen 34 is 50 microns and is used for intercepting powder aggregates and solid impurities in the slurry;
the grooves of the left die 26 and the right die 27 are in nesting fit with the guide table 32 on the bottom die 30, so that the left die 26 and the right die 27 can be tightly closed;
4-15 air exhaust plugs 22 are uniformly distributed at the tops of the left mold 26 and the right mold 27 respectively, and the air exhaust plugs 22 are air exhaust structures of asymmetric air passages which only can allow air to pass through and are used for exhausting air in a mold cavity in a grouting process;
the guide table 32 is used for enabling the left die 26 and the right die 27 to move directionally in the opening and closing process;
the limiting boss 31 is used for limiting the positions of the joint surfaces of the left die 26 and the right die 27;
a sealing bearing 29 is fixed on the shaft sleeve I10, and the left die 26, the right die 27 and the shaft sleeve I10 are connected through the sealing bearing 29, so that liquid leakage of the joint surfaces of the left die 26 and the right die 27 is avoided;
in the process of grouting and pressure maintaining of a mold cavity, under the action of a motor 8, a shaft sleeve I10 rotates (a central shaft 9 and a shaft sleeve II 11 do not move) to drive the metal powder porous matrix pipes 21 to integrally rotate at a constant speed, so that each metal powder porous matrix pipe 21 is ensured to be impacted by the same material liquid, and the coating effect of a film layer is enhanced; after the pressure is released and the slurry 39 falls back, the whole porous metal powder substrate tube 21 continues to rotate for a certain time and then stops, and the left die 26 and the right die 27 are opened.
Porous matrix pipe 21 of metal powder is rotatory by oneself earlier, and back scraper blade 18 carries out rectilinear motion under the drive of center pin 9, and concrete process is: under the action of the motor 8, the shaft sleeve II 11 rotates and drives the pinion 16 and the bull gear 17 to rotate, and the rolling shaft 15 and the supporting shaft 23 rotate along with the rotation, so that the single metal powder porous matrix tube 21 rotates automatically; the central shaft 9 moves under the action of the motor 8, so that the scraper 18 moves horizontally, and directly scrapes and presses the outer wall film layer of the metal powder porous matrix tube 21, thereby effectively controlling the uniformity of the film thickness and further improving the film-substrate bonding strength;
the liquid supply mechanism consists of a sealing cover 36, a slurry pool 38 and a grouting pipe 41, wherein slurry 39 is arranged in the slurry pool 38, the sealing cover 36 is arranged at the top of the slurry pool 38, a feeding port 37 is arranged at one side of the slurry pool 38, the grouting pipe 41 is arranged in the middle of the slurry pool 38, the grouting pipe 41 is in butt joint with the grouting port 33, and the grouting pipe 41 is connected with the grouting port 33 through a sealing gasket 35;
the distance between the bottom end of the grouting pipe 41 and the bottom of the slurry pool 38 is 50 mm;
the number of the grouting pipes 41 depends on the length of the metal powder porous matrix pipe 21, the length of the metal powder porous matrix pipe 21 is not more than 1000mm, 1 grouting pipe 41 is used, the length of the matrix pipe is more than 1000mm and not more than 2000mm, 2 grouting pipes 41 are used, the distance is obtained according to the length of the metal powder porous matrix pipe 21, and the length of the metal powder porous matrix pipe 21 is more than 2000mm of an overlong pipe, and needs to be proved by tests; the grouting pipe 41 and the grouting port 33 are connected through a sealing gasket 35, so that no leakage is caused in the grouting process.
The invention relates to a preparation method of a metal powder porous matrix tube outer wall film layer, wherein the film making process is shown in figure 4, and the specific contents are as follows:
step one, soaking a metal powder porous matrix tube 21 in alcohol; the pore channels of the metal powder porous matrix tube 21 are in a saturated state, so that the positions of the powder particles suspended in the slurry entering the pore channels are shallow under pressure impregnation, a hole sealing state is achieved, the powder particles are uniformly distributed on the outer wall of the metal powder porous matrix tube 21, and the high air permeability of the metal powder porous matrix tube 21 is kept;
secondly, plugging two ports of the metal powder porous matrix tube 21 by using conical plugs, installing and fixing the metal powder porous matrix tube on a supporting shaft 23, installing a filter screen 34, cleaning the inner surface of the die, and closing a left die 26 and a right die 27; 3-8 metal powder porous matrix pipes 21 are installed;
the maximum number of metal powder porous matrix tubes 21 installed increases as the internal space of the die and slurry pool increases;
step three, preparing slurry, wherein the preparation ratio of the polyvinylpyrrolidone to the ethanol solution is 5% -10%; adding the powder into a polyvinylpyrrolidone ethanol solution according to the proportion of 850 g/L-1200 g/L, and injecting slurry into a slurry pool 38 from a feed inlet 37;
setting a pressure parameter, a rack rotation parameter and a stirring parameter;
wherein the pressure is divided into 4 stages: grouting filling, boosting, pressure maintaining and pressure relief, wherein the grouting filling pressure is calculated according to the distance between the liquid level of the slurry and a mold, the mold cavity needs to be filled with the slurry, the pressure maintaining is realized by increasing a certain pressure on the basis of the grouting filling pressure, the grouting and film adsorption process can be accurately controlled by a reasonable pressure value, and powder particles in feed liquid are strongly attached to the outer wall of the metal powder porous matrix tube 21 under the pressure action and are distributed more densely and uniformly;
the stirrer 40 is started once every 30min, and is stirred for 2-5min once at the stirring speed of 30 rad/min;
fifthly, starting grouting, soaking the metal powder porous matrix tube 21 under pressure, and enabling the material rest to rotate in the mold at a constant speed;
step six, releasing pressure, dropping slurry 39, continuously rotating the material rest, opening the left die 26 and the right die 27, checking the impregnation condition of the film layer, enabling the porous metal powder base tube 21 to rotate if the impregnation effect is good, and directly scraping the film layer by the scraper 18 to prepare a wet film on the outer wall of the porous metal powder base tube;
the material rack continues to rotate for 1-3min, and redundant slurry residues are thrown away under the action of centrifugal force;
the film layer is uniformly adsorbed, the surface is smooth, no local non-adsorption or bulge exists, and the impregnation effect is good;
and step seven, drying and sintering the wet film on the outer wall of the metal powder porous matrix tube prepared in the step six to prepare the film layer on the outer wall of the metal powder porous matrix tube.
Example 1
Selecting phi 60X 2.7mm, length 850mm, average pore diameter 25 μm, and air permeability greater than 120m3/m2KPa.h 316L sintered metal powder porous tube as a substrate tube; soaking in 99% industrial alcohol for 5min to saturate the pore channel of the base tube. Mixing polyvinylpyrrolidone, ethanol solution, and 316L 5-7 μm spherical powder at a certain ratio to obtain slurry with viscosity of 10mPa·And s. Setting the grouting mold filling pressure to be 25KPa, the time to be 30s, the pressure rising time to be 5s, the pressure maintaining pressure to be 35KPa, the pressure maintaining time to be 3min and the pressure relief time to be 2 s. The revolution speed of the material rack is 10rad/min, the material rack continues to revolve for 2min after pressure relief, and the rotation speed of the matrix pipe is 60 rad/min. The scraping plate 18 directly scrapes and presses 3.5mm/s, the distance between the scraping plate 18 and the filter element is kept until just contacting the outer wall of the filter element, and the width of the scraping plate 18 in the contact area is 5 mm. Preparing a wet film on the outer wall of the matrix tube, drying for 8 hours at 60 ℃ in an electrothermal blowing drying oven, then placing the matrix tube in a vacuum sintering furnace, preserving heat for 2.5 hours at 400 ℃ for degreasing treatment, preserving heat for 1.5 hours at 1200 ℃ for completing sintering of the film, finally cooling to 60 ℃ along with the furnace, and discharging the film, thus completing the preparation of the outer wall film of the metal powder porous matrix tube.
The detection shows that the thickness of the outer wall film layer of the metal powder porous matrix tube is 20 mu m, the average pore diameter is 6 mu m, and the air permeability is more than 85m3/m2Kpa.h, the film-based bond strength was 20N, and the smoothness of the film layer surface was greatly improved as compared to the substrate tube, as shown in fig. 5.
Example 2
Selecting phi 60X 2.7mm, length 850mm, average pore diameter 25 μm, air permeability greater than 90m3/m2KPa.h 316L sintered metal powder porous tube as a substrate tube; soaking in 99% industrial alcohol for 5min to saturate the pore channel of the base tube. Mixing polyvinylpyrrolidone, ethanol solution, and 316L 5-7 μm spherical powder at a certain ratio to obtain slurry with viscosity of 10mPa·And s. Setting the grouting mold filling pressure to be 25KPa, the time to be 25s, the pressure rising time to be 4s, the pressure maintaining pressure to be 40KPa, the pressure maintaining time to be 3min and the pressure relief time to be 2 s. The revolution speed of the material rest is 10r/min, the material rest continues to revolve for 2min after pressure relief, and the rotation speed of the matrix tube is 60 r/min. The straight scraping speed of the scraper 18 is 3.5mm/s, and the distance between the scraper 18 and the filter core is kept until the scraper just contacts the filter coreThe width of the outer wall, contact area scraper 18 is 5 mm. Preparing a wet film on the outer wall of the matrix tube, drying for 8 hours at 60 ℃ in an electrothermal blowing drying oven, then placing the matrix tube in a vacuum sintering furnace, preserving heat for 2.5 hours at 450 ℃ for degreasing treatment, preserving heat for 1.5 hours at 1200 ℃ for completing sintering of the film, finally cooling to 60 ℃ along with the furnace, and discharging the film, thus completing the preparation of the outer wall film of the metal powder porous matrix tube.
The detection shows that the thickness of the outer wall membrane layer of the metal powder porous substrate tube is 24 mu m, the average pore diameter is 1 mu m, and the air permeability is more than 42m3/m2KPa.h, the bonding strength of the film base is 27N, and the smoothness of the film surface is greatly improved compared with that of the substrate pipe.
Example 3
Selecting phi 60 multiplied by 2.7mm, length 850mm, average aperture 38 mu m, air permeability more than 180m3/m2KPa.h 316L sintered metal powder porous tube as a substrate tube; soaking in 99% industrial alcohol for 5min to saturate the base tube pore canal. Mixing polyvinylpyrrolidone, ethanol solution, and 316L 9-12 μm non-spherical powder at a certain ratio to obtain slurry with viscosity of 10mPa·And s. Setting the grouting mold filling pressure to be 25KPa, the time to be 30s, the pressure rising time to be 5s, the pressure maintaining pressure to be 35KPa, the pressure maintaining time to be 3min and the pressure releasing time to be 2 s. The revolution speed of the material rest is 10r/min, the material rest continues to revolve for 2min after pressure is relieved, and the rotation speed of the base pipe is 60 r/min. The scraper 18 is directly scraped at the speed of 3.5mm/s, the distance between the scraper 18 and the filter element is kept until the scraper just contacts the outer wall of the filter element, and the width of the scraper 18 in the contact area is 5 mm. Preparing a wet film on the outer wall of the matrix tube, drying for 8 hours at 60 ℃ in an electrothermal blowing drying oven, then placing the matrix tube in a vacuum sintering furnace, preserving heat for 2.5 hours at 450 ℃ for degreasing treatment, preserving heat for 1.5 hours at 1200 ℃ for completing sintering of the film, finally cooling to 60 ℃ along with the furnace, and discharging the film, thus completing the preparation of the outer wall film of the metal powder porous matrix tube.
Through detection, the thickness of the outer wall membrane layer of the metal powder porous substrate tube is 25 μm, the average pore diameter is 6 μm, and the air permeability is more than 75m3/m2KPa.h, the bonding strength of the film base is 21N, and the smoothness of the film surface is greatly improved compared with that of the substrate pipe.
Example 4
Selecting phi 60 multiplied by 2.7mm,a length of 850mm, an average pore diameter of 38 μm and an air permeability of more than 180m3/m2KPa.h 316L sintered metal powder porous tube as a substrate tube; soaking in 99% industrial alcohol for 5min to saturate the base tube pore canal. Mixing polyvinylpyrrolidone, ethanol solution, and 316L 9-12 μm non-spherical powder at a certain ratio to obtain slurry with viscosity of 10mPa·And s. Setting the grouting mold filling pressure to be 25KPa, the time to be 25s, the pressure rising time to be 4s, the pressure maintaining pressure to be 40KPa, the pressure maintaining time to be 3min and the pressure releasing time to be 2 s. The revolution speed of the material rest is 10r/min, the material rest continues to revolve for 2min after pressure relief, and the rotation speed of the matrix tube is 60 r/min. The scraping plate 18 directly scrapes and presses 3.5mm/s, the distance between the scraping plate 18 and the filter element is kept until just contacting the outer wall of the filter element, and the width of the scraping plate 18 in the contact area is 5 mm. And (3) preparing a wet film on the outer wall of the substrate tube, drying the wet film for 8 hours at the temperature of 60 ℃ in an electrothermal blowing drying oven, then placing the wet film in a vacuum sintering furnace, preserving heat for 2.5 hours at the temperature of 450 ℃ to carry out degreasing treatment, preserving heat for 1.5 hours at the temperature of 1200 ℃ to finish film layer sintering, and finally cooling the film layer to 60 ℃ along with the furnace to be discharged, thus finishing the preparation of the porous film on the outer wall of the substrate tube.
The detection shows that the thickness of the outer wall membrane layer of the metal powder porous substrate tube is 27 mu m, the average pore diameter is 5 mu m, and the air permeability is more than 70m3/m2KPa.h, the bonding strength of the film base is 28N, and the smoothness of the film layer surface is greatly improved compared with that of the substrate tube.
In the above embodiments of the present invention, the description of each embodiment has its own emphasis, and reference may be made to the related description of other embodiments for parts that are not described in detail in a certain embodiment.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, which is intended to cover any modifications, equivalents, improvements, etc. within the spirit and scope of the present invention.

Claims (10)

1. The device for preparing the metal powder porous matrix tube outer wall film layer is characterized by comprising the following components: the control and power supply mechanism, the pressurization mechanism, the film preparation mechanism and the liquid supply mechanism;
the control and power supply mechanism consists of a control cabinet and a power supply (7), an electric wire (6), a motor (8), a pressure sensor (5), an air cylinder (25) and a stirrer (40), wherein the control cabinet and the power supply (7) are connected with the motor (8), the pressure sensor (5), the air cylinder (25) and the stirrer (40) through the electric wire (6), the motor (8) is connected with a central shaft (9), a shaft sleeve I (10) and a shaft sleeve II (11) through the electric wire (6), and the central shaft (9) is arranged on the ground through a ground pillar (24);
the pressurizing mechanism consists of a compressed air tank (1), an air valve (2), a pressure gauge (3) and an air pipe (4), wherein the air valve (2) and the pressure gauge (3) are arranged on the compressed air tank (1), and the air pipe (4) is connected with the slurry pool (38) and the compressed air tank (1) through a joint;
the film making mechanism comprises a material rack and a mold, wherein the material rack is arranged in the mold, and a central shaft (9) penetrates through the mold;
the liquid supply mechanism is composed of a sealing cover (36), a slurry pool (38) and a grouting pipe (41), slurry (39) is arranged in the slurry pool (38), the sealing cover (36) is arranged at the top of the slurry pool (38), a feeding port (37) is arranged on one side of the slurry pool (38), the grouting pipe (41) is arranged in the middle of the slurry pool (38), the grouting pipe (41) is in butt joint with the grouting port (33), and the grouting pipe (41) and the grouting port (33) are connected through a sealing gasket (35).
2. The apparatus for preparing the outer wall membrane layer of the metal powder porous matrix tube according to claim 1, wherein the stirrer (40) is composed of a stirring motor, a stirring shaft and a stirring blade.
3. The device for preparing the film layer on the outer wall of the metal powder porous matrix tube according to claim 1, wherein a shaft sleeve I (10) and a shaft sleeve II (11) are sequentially arranged on the central shaft (9) from inside to outside, the central shaft (9), the shaft sleeve I (10) and the shaft sleeve II (11) are connected through a shaft sleeve spacing device (12), a large gear (17) and a bearing support rod (14) are arranged on the shaft sleeve II (11), a bearing (13) is arranged on the bearing support rod (14), a small gear (16) is meshed with the large gear (17), the bearing (13) is connected with the small gear (16) through a rolling shaft (15), a nut seat (19) is arranged on the central shaft (9), and a scraper (18) is arranged on the nut seat (19) and a support guide rail (20);
the material rest consists of a scraper (18), a supporting guide rail (20), a metal powder porous matrix tube (21) and a supporting shaft (23), wherein bearings (13) and bearing supporting rods (14) are arranged at two ends of the material rest, the bearings (13) are arranged on the bearing supporting rods (14), the bearing supporting rods (14) are arranged on a shaft sleeve I (10), and the metal powder porous matrix tube (21) is connected with the supporting shaft (23) through the bearings (13); the mold consists of an exhaust plug (22), a left mold (26), a right mold (27) and a bottom mold (30), wherein the bottom mold (30) is provided with a grouting opening (33), the left mold (26) and the right mold (27) are arranged on a guide table (32), the guide table (32) is fixed on the bottom mold (30), and a limiting boss (31) is arranged in the middle of the guide table (32); grooves are carved at corresponding positions of the left die (26) and the right die (27), sealing buttons (28) are arranged on the left die (26) and the right die (27), and air exhaust plugs (22) are arranged at the tops of the left die (26) and the right die (27); the left die (26) and the right die (27) are opened, and the rolling shaft (15) is connected with the supporting shaft (23).
4. The apparatus for preparing the membrane layer on the outer wall of the metal powder porous matrix tube according to claim 3, wherein the bottom surface of the bottom mold (30) is flush with the top end of the grouting tube (41).
5. The device for preparing the membrane layer on the outer wall of the metal powder porous matrix tube as claimed in claim 1, wherein the central portion of the central shaft (9) is a lead screw.
6. The apparatus for preparing the membrane layer on the outer wall of the metal powder porous matrix tube according to claim 1, wherein the injection port (33) is provided with a screen (34), and the aperture of the screen (34) is 50 μm.
7. The device for preparing the membrane layer on the outer wall of the metal powder porous matrix tube as claimed in claim 1, wherein 4-15 vent plugs (22) are uniformly distributed at the top of each of the left die (26) and the right die (27).
8. The apparatus for preparing the outer wall membrane layer of the metal powder porous matrix tube according to claim 1, wherein the distance between the bottom end of the grouting tube (41) and the bottom of the slurry pool (38) is 50 mm.
9. A preparation method of a metal powder porous matrix tube outer wall film layer is characterized by comprising the following steps:
step one, soaking a metal powder porous matrix tube (21) by alcohol;
secondly, plugging two ports of the metal powder porous matrix tube (21) by using conical plugs, installing and fixing the metal powder porous matrix tube on a supporting shaft (23), installing a filter screen (34), cleaning the inner surface of a mold, and closing a left mold (26) and a right mold (27); 3-8 metal powder porous matrix pipes (21) are installed;
step three, preparing slurry, wherein the preparation ratio of the polyvinylpyrrolidone to the ethanol solution is 5% -10%; adding the powder into a polyvinylpyrrolidone ethanol solution according to the proportion of 850 g/L-1200 g/L, and injecting the slurry into a slurry pool (38) from a feed inlet (37);
setting pressure parameters, rack rotation parameters and stirring parameters;
step five, starting grouting, dipping the metal powder porous matrix tube (21) under pressure, and enabling the material rest to rotate at a constant speed in the mold;
step six, releasing pressure, enabling the slurry (39) to fall back, continuously rotating the material rack, opening a left die (26) and a right die (27), checking the impregnation condition of the film layer, enabling the porous metal powder base tube (21) to rotate if the impregnation effect is good, and directly scraping the film layer by a scraper (18) to prepare a wet film on the outer wall of the porous metal powder base tube;
and step seven, drying and sintering the wet film on the outer wall of the metal powder porous matrix tube prepared in the step six to prepare the film layer on the outer wall of the metal powder porous matrix tube.
10. The method as claimed in claim 9, wherein the stirrer (40) of the fourth step is started every 30min, and is stirred for 2-5min at a stirring speed of 30 rad/min.
CN202210720615.6A 2022-06-24 2022-06-24 Method and device for preparing outer wall film layer of metal powder porous matrix tube Pending CN114769597A (en)

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Publication number Priority date Publication date Assignee Title
US4088576A (en) * 1976-12-13 1978-05-09 Mott Lambert H Method of manufacture of tubular inertial filter
US4719058A (en) * 1985-04-12 1988-01-12 Ngk Insulators, Ltd. Process of producing multiple-layer filter medium
EP0419799A2 (en) * 1989-07-28 1991-04-03 Pall Corporation Slip casting process for preparing metal filters
EP0446664A1 (en) * 1990-03-14 1991-09-18 Asea Brown Boveri Ag Process for the production of components with a complicated profile by forming a dense product from pourable powder
JP2000288324A (en) * 1999-02-01 2000-10-17 Ngk Insulators Ltd Production of filter containing ceramic porous membrane as separation membrane
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CN111254755A (en) * 2020-01-17 2020-06-09 西部宝德科技股份有限公司 Centrifugal auxiliary vacuum filtration forming system of ceramic fiber perforated pipe

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