CN113058440B - Preparation method of tubular powder mesh composite porous metal film - Google Patents

Preparation method of tubular powder mesh composite porous metal film Download PDF

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CN113058440B
CN113058440B CN202110386191.XA CN202110386191A CN113058440B CN 113058440 B CN113058440 B CN 113058440B CN 202110386191 A CN202110386191 A CN 202110386191A CN 113058440 B CN113058440 B CN 113058440B
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powder
metal film
mesh composite
composite porous
porous metal
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CN113058440A (en
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曹卜元
吴引江
王耀辉
成凯
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Western Baode Technologies Co ltd
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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
    • B01D67/0039—Inorganic membrane manufacture
    • 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
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
    • 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
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • 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
    • B01D69/04—Tubular membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/022—Metals

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  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)
  • Filtering Materials (AREA)

Abstract

The invention discloses a preparation method of a tubular powder mesh composite porous metal film, which comprises the following steps: 1. uniformly mixing metal powder with a plasticizer, a thickening agent and an organic solvent according to a certain proportion to prepare high-viscosity slurry; 2. extruding the high-viscosity slurry into a strip-shaped film blank through a slit-shaped die opening by using an extruder, conveying the strip-shaped film blank to a rolling mill, and rolling and compounding the strip-shaped film blank with a single-layer or multi-layer sintered metal wire mesh to prepare a powder mesh composite metal film blank; 3. preparing the powder mesh composite metal film blank into a tube by using a tube coiling machine, degreasing and sintering at high temperature in a sintering furnace to prepare a tube-type powder mesh composite metal film, and finally performing straight seam welding to finish the preparation. The preparation process of the invention has simple flow and low cost, and the prepared tubular powder mesh composite porous metal membrane has large permeation flux and controllable precision, and can be widely applied to liquid-solid and gas-solid separation in the fields of petrochemical industry, coal chemical industry and environmental protection.

Description

Preparation method of tubular powder mesh composite porous metal film
Technical Field
The invention belongs to the technical field of filter materials, and particularly relates to a preparation method of a tubular powder mesh composite porous metal film.
Background
The porous metal membrane separation material is widely applied in the fields of environmental protection, petrochemical industry, coal chemical industry and other industrial fields. At present, a porous metal film mainly uses a powder sintered porous material as a support body, and a gradient composite control layer is prepared on the surface by processes such as spraying or centrifuging. However, the powder sintered porous material support has low permeability coefficient, complex preparation process, high processing difficulty and high cost. Therefore, it is necessary to develop a porous metal membrane separation material with high permeability, low cost and high precision.
Disclosure of Invention
The invention aims to provide a preparation method of a tubular powder mesh composite porous metal membrane, which solves the problems of low permeation flux, high manufacturing cost and complex preparation process of the existing powder sintering gradient composite porous metal membrane.
The technical scheme adopted by the invention is as follows: a preparation method of a tubular powder mesh composite porous metal film comprises the following steps:
step 1, uniformly mixing a thickening agent and an organic solution according to a mass ratio of 1;
step 2, uniformly mixing a plasticizer with the mixed solution A obtained in the step 1 according to the mass ratio of 1;
step 3, mixing and stirring the metal powder and the mixed liquid B obtained in the step 2 according to the mass ratio of 5-8;
step 4, pouring the high-viscosity thick paste system obtained in the step 3 into an extruder, extruding a metal film blank with the width of 500-1000 mm and the thickness of 100-300 mu m from a slit-shaped die opening, conveying the metal film blank to a two-roll mill, and rolling and compounding the metal film blank with a multi-layer or single-layer sintered metal wire mesh to form an asymmetric powder mesh composite porous metal film blank;
and 5, preparing the asymmetric powder mesh composite porous metal film blank obtained in the step 4 into a tubular film by using a tube coiling machine, then putting the tubular film blank into a sintering furnace for organic matter removal and high-temperature sintering to obtain the powder mesh composite porous metal film, and then performing straight seam welding to obtain the tubular powder mesh composite porous metal film.
The present invention is also characterized in that,
the thickening agent in the step 1 is polyvinyl butyral, and the organic solution is one of ethanol, isopropanol, butanol or butanone.
The plasticizer in the step 2 is one of dibutyl phthalate, glycerol or dioctyl phthalate.
The metal powder in step 3 is made of 304 stainless steel, 316L stainless steel, 310s stainless steel and Fe 3 One of Al alloy powder, nickel-based high-temperature alloy, iron-based high-temperature alloy, copper powder, nickel powder or titanium powder, wherein the granularity of the metal powder is less than or equal to 25 mu m.
The specification of the slit die in step 4 is 500 mm. Times.100. Mu.m, 500 mm. Times.200. Mu.m, 500 mm. Times.300. Mu.m, 1000 mm. Times.100. Mu.m, 1000 mm. Times.200. Mu.m, or 1000 mm. Times.300. Mu.m.
In step 4, the material of the multi-layer or single-layer sintered wire mesh is one of 304L stainless steel, 316L stainless steel, cu, feCrAl or 310S stainless steel.
In the step 4, the filtering precision of the multilayer or single-layer sintered metal wire mesh is 20-60 mu m, and the multilayer sintered metal wire mesh is compounded by 3-10 layers.
And in the step 4, the rolling force of the two rolling mills is controlled to be 50-100T.
Step 5, putting the mixture into a sintering furnace for removing organic matters, wherein the temperature is 500-550 ℃, and keeping the temperature for 120-180 min; the temperature of high-temperature sintering is 1000-1250 ℃, and the temperature is kept for 40-60 min.
And 5, the sintering furnace in the step 5 is a hydrogen atmosphere sintering furnace or a vacuum sintering furnace.
The invention has the beneficial effects that:
1. the invention compositely rolls the extrusion film blank and the sintering metal wire mesh, and prepares the powder mesh composite porous metal film after pipe coiling, sintering and welding, and has simple process flow and low manufacturing cost;
2. the penetration flux of the straight channel structure of the metal sintering wire mesh support body is far higher than that of the powder sintering porous support body, and the prepared powder mesh composite porous metal membrane has higher penetration flux and controllable precision.
Drawings
FIG. 1 is a process flow diagram of a method for preparing a tubular powder mesh composite porous metal membrane according to the present invention;
FIG. 2 is a surface local magnified electron microscope photograph of a powder mesh composite metal film prepared by the method for preparing a tubular powder mesh composite porous metal film of the present invention;
FIG. 3 is a sectional electron microscope photograph of a powder mesh composite porous metal film prepared by the method of the present invention.
In the figure, 1, an extruder, 2, a film blank, 3, two roll mills, 4, a wire mesh, 5, a tube rolling machine.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a preparation method of a tubular powder mesh composite porous metal film, which comprises the steps of adding metal powder into a mixture added with a plasticizer, a thickening agent and an organic solution as shown in figure 1, stirring and dispersing, and finally preparing a high-viscosity slurry system. Pouring the prepared high-viscosity slurry system into an extruder 1 with a head provided with a slit die orifice, extruding a film blank 2 from the head, transferring the film blank to a two-roll mill 3, rolling and compounding the film blank with a single-layer or multi-layer sintered metal wire mesh 4 porous material to form an asymmetric powder mesh composite film blank, preparing the film blank into a tubular film by a tube rolling machine 5, and degreasing and sintering the tubular film blank to prepare the tubular powder mesh composite porous metal film with high permeation flux and controllable filtration precision. The method specifically comprises the following steps:
step 1, uniformly mixing a thickening agent and an organic solution according to a mass ratio of 1; wherein, the thickening agent is preferably polyvinyl butyral, and the organic solution is preferably one of ethanol, isopropanol, butanol or butanone;
step 2, uniformly mixing the plasticizer and the mixed solution A obtained in the step 1 according to the mass ratio of 1; wherein, the plasticizer is preferably one of dibutyl phthalate, glycerol or dioctyl phthalate;
step 3, mixing and stirring the metal powder and the mixed liquid B obtained in the step 2 according to the mass ratio of 5-8; the material of the metal powder is preferably 304 stainless steel, 316L stainless steel, 310s stainless steel, or Fe 3 One of Al alloy powder, nickel-based high-temperature alloy, iron-based high-temperature alloy, copper powder, nickel powder or titanium powder, wherein the granularity of the metal powder is less than or equal to 25 mu m;
step 4, pouring the high-viscosity slurry system obtained in the step 3 into an extruder, and extruding a metal film blank with the width of 500-1000 mm and the thickness of 100-300 microns from a slit-shaped die opening, wherein the slit-shaped knife edge is provided with a plurality of dies with different sizes, including dies with various specifications and sizes, such as 500mm multiplied by 100 microns, 500mm multiplied by 200 microns, 500mm multiplied by 300 microns, 1000mm multiplied by 100 microns, 1000mm multiplied by 200 microns or 1000mm multiplied by 300 microns; conveying the metal wire mesh to a two-roll mill, controlling the rolling force at 50-100T, and rolling and compounding the metal wire mesh with a multi-layer or single-layer sintered metal wire mesh, wherein the material of the multi-layer or single-layer sintered metal wire mesh is preferably one of 304L stainless steel, 316L stainless steel, cu, feCrAl and 310S stainless steel; the filtering precision of the multilayer or single-layer sintered metal wire mesh is 20-60 mu m, and the multilayer sintered metal wire mesh is compounded by 3-10 layers to form an asymmetric powder mesh composite porous metal film blank;
step 5, preparing the asymmetric powder mesh composite porous metal film blank obtained in the step 4 into a tubular film by using a tube coiling machine, then putting the tubular film into a hydrogen atmosphere sintering furnace or a vacuum sintering furnace for organic matter removal and high-temperature sintering, wherein the temperature for organic matter removal is 500-550 ℃, and keeping the temperature for 120-180 min; the temperature of high-temperature sintering is 1000-1250 ℃, the temperature is kept for 40-60 min, the powder mesh composite porous metal film is prepared, then straight seam welding is carried out, and finally the tubular powder mesh composite porous metal film is prepared.
Through the way, as shown in figure 1, the process flow chart of the tubular powder mesh composite porous metal film preparation method is simple in process and high in efficiency; fig. 2 and fig. 3 are electron micrographs of the surface and the section of the tubular powder mesh composite porous metal film prepared by the invention, good sintering wells are formed among metal powder, good metallurgical bonding is formed, the strength is high, the section shows an obvious asymmetric structure of the wire mesh, a metal powder control layer is embedded in a mesh structure of the sintering metal wire, good mechanical occlusion is formed, and the bonding strength of the film layer is high.
Example 1
1. Preparing a PVB ethanol solution according to the mass ratio of 1.
2. Mixing 316L powder with the average particle size of 10 mu m and the mixed liquid according to the mass ratio of 5, slowly adding metal powder, and stirring to obtain a viscous slurry system;
3. pouring the viscous slurry system into an extruder, extruding a thin film blank with the length and the width of 1000mm multiplied by 500mm from a slit type die opening with the size of 500mm multiplied by 200 mu m under the pushing of a screw rod, and rolling and compounding the thin film blank with a 316L stainless steel sintered metal wire mesh with the size of 1000mm multiplied by 500mm, 3 layers and the filtering precision of 20 mu m under the action of the rolling force of 50T by a rolling mill to prepare a powder mesh composite metal film blank;
4. processing the powder mesh composite metal film blank into a tube by using a tube coiling machine, loading the tube into a hydrogen atmosphere sintering furnace, heating to 500 ℃ at the speed of 5 ℃/min, preserving heat for 180min to remove organic matters, heating to 1000 ℃ at the speed of 10 ℃/min, preserving heat for 60min to form a finished sintering trap among metal powder, and preparing the powder mesh composite metal film with the average pore diameter of 2 mu m after heat preservation.
The surface and cross-section of the powder mesh composite metal film prepared in this example were partially magnified by electron microscopy as shown in fig. 2 and 3, and the pore size distribution was uniform and the porosity was high. The maximum pore diameter of the powder mesh composite porous metal film of the embodiment is 5 μm, the average pore diameter is 2 μm, and the permeability coefficient is 250m measured according to the national standard GB/T5429-1985' determination of pore diameters of permeable sintered metal materials and bubble samples 2 .kPa.h。
Example 2
1. Preparing a PVB isopropanol solution according to a mass ratio of 1.
2. Mixing 316L of powder with the average particle size of 20 mu m and the mixed liquid according to the mass ratio of 6;
3. pouring the viscous slurry system into an extruder, extruding a thin film blank with the length and width of 1000mm multiplied by 1000mm from a slit-shaped die opening with the size of 1000mm multiplied by 300 mu m under the pushing of a screw rod, and rolling and compounding the thin film blank with a 316L stainless steel sintered wire mesh with the size of 1000mm multiplied by 1000mm, 5 layers and the filtering precision of 50 mu m under the action of the rolling force of 100T by a rolling mill to prepare a powder mesh composite metal film blank;
4. processing the powder mesh composite metal film blank into a tube by using a tube coiling machine, loading the tube into a hydrogen atmosphere sintering furnace, heating to 500 ℃ at the speed of 5 ℃/min, preserving heat for 180min to remove organic matters, heating to 1100 ℃ at the speed of 10 ℃/min, preserving heat for 50min to form a finished sintering trap among metal powder, and obtaining the powder mesh composite metal film with the average aperture of 5 mu m after heat preservation.
Example 3
1. Preparing a PVB ethanol solution according to a mass ratio of 1.
2. Fe with an average particle size of 15 μm 3 Mixing Al powder and the mixed liquid according to the mass ratio of 8;
3. pouring the viscous slurry system into an extruder, extruding a film blank with the length and width of 500mm multiplied by 500mm from a slit-shaped die opening with the size of 500mm multiplied by 100 mu m under the pushing of a screw, and rolling and compounding the film blank with a FeCrAl sintered metal wire mesh with the size of 500mm multiplied by 500mm, 10 layers of composite and the filtering precision of 30 mu m under the action of the rolling force of 80T by a rolling mill to prepare a powder mesh composite metal film blank;
4. processing the powder mesh composite metal film blank into a tube by using a tube coiling machine, loading the tube into a hydrogen atmosphere sintering furnace, heating to 500 ℃ at the speed of 5 ℃/min, preserving heat for 180min to remove organic matters, heating to 1200 ℃ at the speed of 10 ℃/min, preserving heat for 45min to form a finished sintering trap among metal powder, and preparing the powder mesh composite metal film with the average pore diameter of 3 mu m after heat preservation.
Example 4
1. Preparing a butanol solution of PVB according to a mass ratio of 1.
2. Mixing 310S powder with the average particle size of 20 mu m and the mixed liquid according to the mass ratio of 6;
3. pouring the viscous slurry system into an extruder, extruding a thin film blank with the length and width of 2000mm multiplied by 1000mm from a slit-shaped die opening with the size of 1000mm multiplied by 200 mu m under the pushing of a screw, and rolling and compounding the thin film blank with a 310S sintered wire mesh with the size of 2000mm multiplied by 1000mm, 3 layers of composite and the filtering precision of 35 mu m under the action of the rolling force of 100T by a rolling mill to prepare a powder mesh composite metal film blank;
4. processing the powder mesh composite metal film blank into a tube by using a tube coiling machine, loading the tube into a hydrogen atmosphere sintering furnace, heating to 550 ℃ at the speed of 5 ℃/min, preserving heat for 120min to remove organic matters, heating to 1250 ℃ at the speed of 5 ℃/min, preserving heat for 40min to form a finished sintering trap among metal powder, and preparing the powder mesh composite metal film with the average pore diameter of 12 mu m after heat preservation.
Example 5
1. Preparing a butanone solution of PVB according to a mass ratio of 1.
2. Mixing 304L of powder with the average particle size of 12 μm and the mixed liquid according to the mass ratio of 5;
3. pouring the viscous slurry system into an extruder, extruding a thin film blank with the length and width of 2000mm multiplied by 500mm from a slit die opening with the size of 500mm multiplied by 100 mu m under the pushing of a screw rod, and rolling and compounding the thin film blank with a single-layer sintered metal wire mesh with the size of 2000mm multiplied by 500mm and the filtering precision of 60 mu m and 304L under the action of the rolling force of 60T by a rolling mill to prepare a powder mesh composite metal film blank;
4. processing the powder mesh composite metal film blank into a tube by using a tube coiling machine, loading the tube into a hydrogen atmosphere sintering furnace, heating to 530 ℃ at a speed of 5 ℃/min, keeping the temperature for 150min to remove organic matters, heating to 1100 ℃ at a speed of 10 ℃/min, keeping the temperature for 50min to form a sintering trap among metal powder, and obtaining the powder mesh composite metal film with the average aperture of 4 mu m after the heat preservation is finished.

Claims (7)

1. The preparation method of the tubular powder mesh composite porous metal film is characterized by comprising the following steps of:
step 1, uniformly mixing a thickening agent and an organic solution according to a mass ratio of 1;
step 2, uniformly mixing a plasticizer with the mixed solution A obtained in the step 1 according to a mass ratio of 1;
step 3, mixing and stirring the metal powder and the mixed liquid B obtained in the step 2 according to the mass ratio of 5-8;
step 4, pouring the high-viscosity thick paste system obtained in the step 3 into an extruder, extruding a metal film blank with the width of 500-1000 mm and the thickness of 100-300 mu m from a slit-shaped die opening, conveying the metal film blank to a two-roll mill, controlling the rolling force of the two-roll mill to be 50-100T, and rolling and compounding the metal film blank with a multilayer or single-layer sintered metal wire mesh, wherein the filtering precision of the multilayer or single-layer sintered metal wire mesh is 20-60 mu m, and the multilayer sintered metal wire mesh is compounded with 3-10 layers to form an asymmetric powder mesh composite porous metal film blank;
and 5, preparing the asymmetric powder mesh composite porous metal film blank obtained in the step 4 into a tubular film by using a tube coiling machine, then putting the tubular film into a sintering furnace to carry out organic matter removal and high-temperature sintering to obtain a powder mesh composite porous metal film, carrying out straight seam welding, and finally preparing to obtain the tubular powder mesh composite porous metal film.
2. The method for preparing the tubular powder mesh composite porous metal membrane as claimed in claim 1, wherein the organic solution in the step 1 is one of ethanol, isopropanol, butanol or butanone.
3. The method for preparing a tubular powder mesh composite porous metal film according to claim 1, wherein the metal powder in the step 3 is 304 stainless steel, 316L stainless steel, 310s stainless steel or Fe 3 One of Al alloy powder, nickel-based high-temperature alloy, iron-based high-temperature alloy, copper powder, nickel powder or titanium powder, wherein the granularity of the metal powder is less than or equal to 25 mu m.
4. The method for preparing a tubular powder mesh composite porous metal film according to claim 1, wherein the specification size of the slit type die opening in the step 4 is 500mm x 100 μm, 500mm x 200 μm, 500mm x 300 μm, 1000mm x 100 μm, 1000mm x 200 μm or 1000mm x 300 μm.
5. The method for preparing a tubular powder mesh composite porous metal membrane as claimed in claim 1, wherein the material of the multi-layer or single-layer sintered wire mesh in step 4 is one of 304L stainless steel, 316L stainless steel, cu, feCrAl or 310S stainless steel.
6. The method for preparing the tubular powder mesh composite porous metal film according to claim 1, wherein the temperature for removing organic matters in the step 5 in a sintering furnace is 500-550 ℃, and the temperature is kept for 120-180 min; the temperature of high-temperature sintering is 1000-1250 ℃, and the temperature is kept for 40-60 min.
7. The method for preparing a tubular powder mesh composite porous metal film according to claim 1, wherein the sintering furnace in the step 5 is a hydrogen atmosphere sintering furnace or a vacuum sintering furnace.
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CN114642920A (en) * 2022-05-20 2022-06-21 鑫膜新材料科技(西安)有限公司 Unsupported metal porous filter tube and preparation method thereof
CN115446309B (en) * 2022-08-29 2024-04-23 华南理工大学阳江研究院 Preparation method of concentric-circle-structured strip steel core multilayer composite stainless steel piece
CN116196771A (en) * 2023-04-28 2023-06-02 成都华之煜新材料有限公司 Preparation method of asymmetric porous metal film with high porosity

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