CN112569685B - Preparation method of composite porous film - Google Patents
Preparation method of composite porous film Download PDFInfo
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- CN112569685B CN112569685B CN201910938710.1A CN201910938710A CN112569685B CN 112569685 B CN112569685 B CN 112569685B CN 201910938710 A CN201910938710 A CN 201910938710A CN 112569685 B CN112569685 B CN 112569685B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/30—Particle separators, e.g. dust precipitators, using loose filtering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
- B01D46/543—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
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Abstract
The invention discloses a preparation method of a composite porous film, which comprises the following steps: (1) Obtaining first slurry, and then attaching the first slurry to the support body, so that the pores of the support body are partially or completely filled with the first slurry, and a first precursor is obtained; (2) Obtaining second slurry, attaching the second slurry to one side of the first precursor, and drying to obtain a second precursor; (3) Sintering, so that the first slurry is converted into a first filter layer, and the second slurry is converted into a second filter layer, thus obtaining a third precursor; (4) Loading an alloy film anticorrosive layer on the outer surface and/or pore surface of the third precursor to obtain the composite porous film; the first slurry and the second slurry adopt the same raw material powder. The alloy film anticorrosive layer can protect the whole porous film, prevent local corrosion phenomenon from happening when certain low temperature working conditions are in service, and further prolong the service life.
Description
Technical Field
The invention relates to the technical field of filter materials, in particular to a preparation method of a composite porous film.
Background
At present, the preparation method of the porous film comprises the following steps: (1) obtaining a support and slurry; (2) loading the slurry on a support; and (3) drying and sintering.
The process has the following problems:
(1) The support body mainly adopts plain metal screen mesh, the cost is higher, and the strength of the prepared film is lower.
(2) The slurry on the support body is unevenly distributed, so that defects exist in the appearance and the performance of the product.
(3) When the porous film is in service under certain low-temperature working conditions, local corrosion (acid condensation) phenomenon can occur, and the service life of the porous film is reduced.
Disclosure of Invention
A first object of the present invention is to provide a composite porous film to solve the problems of low strength and poor corrosion resistance of the porous film in the prior art.
The second object of the present invention is to provide a method for preparing a composite porous film, which solves the problems of low strength, poor corrosion resistance and appearance and performance defects caused by uneven slurry distribution of the porous film in the prior art.
In order to achieve the above object, the present invention provides a composite porous membrane comprising a first filter structure and a second filter structure; the first filtering structure comprises a supporting body and a first filtering layer, and the pores of the supporting body are partially or completely filled by the first filtering layer; the second filter structure comprises a second filter layer positioned on one side of the first filter structure; the composite porous film further comprises an anti-corrosion layer; the anti-corrosion layer comprises a first anti-corrosion layer arranged on the pore surfaces of the first filtering structure and the second filtering structure and/or a second anti-corrosion layer arranged on the outer surfaces of the first filtering structure and the second filtering structure.
The first filter layer and the second filter layer are connected into a whole, so that the strength of the porous film can be obviously improved; when the first filter layer is combined with the support body, the second filter layer is arranged, so that the apparent mass of the second filter layer can be improved; the first anti-corrosion layer and the second anti-corrosion layer can protect the whole porous film, so that the phenomenon of local corrosion (acid condensation) can be prevented when certain low-temperature working conditions are in service, and the service life is further prolonged. When the first anti-corrosion layer and the second anti-corrosion layer are simultaneously arranged, the first anti-corrosion layer and the second anti-corrosion layer cooperate, so that the whole porous film can be fully protected.
Further, the anti-corrosion layer further comprises a third anti-corrosion layer arranged between the support body and the first filter layer. Therefore, the third anti-corrosion layer can effectively prevent the support body from being corroded, and the service life is prolonged;
further, the third anti-corrosion layer is a metal plating layer arranged on the surface of the support body. Therefore, the anti-corrosion effect is good and the anti-corrosion agent is easy to obtain.
Further, the metal plating layer is a nickel layer, a zinc layer or a chromium layer. The metal plating layer is preferably a nickel layer, is easy to obtain and has good corrosion resistance.
Further, the first anti-corrosion layer and the second anti-corrosion layer are alloy films, non-metal oxide films or metal oxide films.
Further, the alloy film is a Ni-P alloy film; the non-metal oxide film is SiO 2 A film; the metal oxide film is Al 2 O 3 A film.
Further, the thickness of the first anti-corrosion layer is 10-20 mu m; the thickness of the second anti-corrosion layer is 10-20 mu m. Therefore, better air flux can be maintained on the premise of ensuring better corrosion resistance, and the filtering effect is improved.
Further, in the thickness direction of the support body, the first filter layers are symmetrically distributed. Therefore, the first filter layer and the supporting body have stronger binding force and more stable structure.
Further, the pore size of the first filter structure is larger than the pore size of the second filter structure. Therefore, in the thickness direction of the composite porous film, the pore diameters are distributed in a gradient manner, the air flux is larger, and the filtering efficiency can be remarkably improved.
Further, the pore diameter of the first filtering structure is 30-50 μm, and the pore diameter of the second filtering structure is 15-25 μm. Therefore, the filter has high filter precision and high filter efficiency.
Further, the thickness of the second filter layer is 0.05-0.3 mm; the thickness of the support body is 0.05-1 mm. Thereby, a smaller filtration pressure is ensured.
In order to achieve the above object, the preparation method of the first composite porous film provided by the invention comprises the following steps:
(1) Obtaining first slurry, and then attaching the first slurry to the support body, so that the pores of the support body are partially or completely filled with the first slurry, and a first precursor is obtained;
(2) Obtaining second slurry, attaching the second slurry to one side of the first precursor, and drying to obtain a second precursor;
(3) Sintering, so that the first slurry is converted into a first filter layer, and the second slurry is converted into a second filter layer, thus obtaining a third precursor;
(4) Loading a metal oxide film anticorrosive layer on the outer surface and/or pore surface of the third precursor to obtain the composite porous film;
pore diameter: the first filter structure is greater than the second filter structure.
The first filter layer and the second filter layer are connected into a whole, so that the strength of the porous film can be obviously improved; when the first filter layer is combined with the support body, the second filter layer is arranged, so that the apparent mass of the second filter layer can be improved; the first anti-corrosion layer and the second anti-corrosion layer can protect the whole porous film, so that the phenomenon of local corrosion (acid condensation) can be prevented when certain low-temperature working conditions are in service, and the service life is further prolonged. When the first anti-corrosion layer and the second anti-corrosion layer are provided at the same time, the first anti-corrosion layer and the second anti-corrosion layer cooperate, so that the whole porous film can be fully protected; in the thickness direction of the porous film, the pore diameters are distributed in a gradient way, so that the gas flux is larger, and the filtering efficiency can be remarkably improved.
Further, viscosity: the first slurry > the second slurry. The higher the viscosity of the slurry, the lower the content of the raw material powder, and the larger the pore diameter of the obtained filter layer, so that the pore diameter of the porous film is changed in a gradient manner by controlling the viscosity of the slurry, and the bonding force between the first filter layer and the support body is stronger.
Further, the viscosity of the first slurry is 5000-15000 mPa.s; the viscosity of the second slurry is 40-80 mPas. Therefore, the proper slurry fluidity can ensure better product quality, is beneficial to reducing defects such as holes, concave-convex differences and the like, and prolongs the service life.
Further, in the step (1), the first slurry is attached to the support body by adopting a doctor blade coating mode; and (2) attaching the second slurry to one side of the first precursor in a spraying mode. Therefore, the first slurry can fully fill the pores of the support body by adopting a doctor blade coating mode, so that the binding force between the first filter layer and the support body is improved, and meanwhile, the surface of the obtained first filter structure is flat, and the second filter layer with uniform distribution is facilitated to be obtained. When the viscosity of the first sizing agent is larger than that of the second sizing agent, the production efficiency can be improved to the greatest extent by the aid of the cooperation mode of blade coating and spraying, and the product quality is guaranteed.
Further, the first slurry and the second slurry adopt the same raw material powder. Therefore, the binding force between the first filter layer and the second filter layer is improved.
Further, the first slurry employs a multi-component binder; the second slurry employs a one-component binder. When the same binder is used, the higher the viscosity of the slurry, the higher the binder usage amount, the lower the raw material powder usage amount, and the larger the pores of the produced porous film; when the multi-component adhesive is adopted, for example, the multi-component adhesive consisting of the adhesive with high price and good bonding effect and the adhesive with low price and poor bonding effect is beneficial to controlling the use amount of raw material powder, controlling the cost and keeping high filtering precision.
Further, the binder is selected from CMC (sodium carboxymethyl cellulose), SBR (styrene butadiene rubber) and PVA (polyvinyl alcohol).
Further, the thickness of the metal oxide film is 10 to 20 μm. Therefore, the porous membrane has corrosion resistance and can improve the filtering precision of the porous membrane.
Further, the metal oxide film is Al 2 O 3 A film. Al (Al) 2 O 3 The film has the characteristics of high toughness, easy processing, high corrosion resistance, high wear resistance and the like of ceramic materials.
Further, the Al 2 O 3 The film is burned by Al sol attached to the outer surface of the third precursor and/or the pore surfaceThe junction is obtained. Thereby Al is provided with 2 O 3 The film has strong binding force with the third precursor, and the thickness is easy to control.
In order to achieve the above object, the preparation method of the second composite porous film provided by the invention comprises the following steps:
(1) Preparing a first slurry with the viscosity of 5000-15000 mPa.s by taking alloy powder as raw material powder and CMC and SBR as binders, and then enabling a support body carrying the first slurry to pass through a gap between two scrapers at the speed of 3-5 m/min to obtain a first precursor;
(2) Preparing second slurry with the viscosity of 40-80 mPas by taking alloy powder as raw material powder and PVA as a binder, spraying the second slurry on one side of the first precursor, and drying to obtain a second precursor;
(3) Rolling the second precursor;
(4) Sintering the rolled second precursor: the first stage is heat-preserving for 60-90 min at 120-250 ℃, the second stage is heat-preserving for 60-120 min at 500-600 ℃, and the third stage is heat-preserving for 90-180 min at 900-1150 ℃ to obtain a third precursor;
(5) Soaking the third precursor in Al sol, taking out, sintering at 450-650 deg.c to convert Al sol into Al 2 O 3 And forming a first anticorrosive layer on the pore surfaces of the third precursor and forming a second anticorrosive layer on the outer surface of the third precursor to obtain the composite porous film.
In order to achieve the above object, the third preparation method of the composite porous film provided by the invention comprises the following steps:
(1) Obtaining first slurry, and then attaching the first slurry to the support body, so that the pores of the support body are partially or completely filled with the first slurry, and a first precursor is obtained;
(2) Obtaining second slurry, attaching the second slurry to one side of the first precursor, and drying to obtain a second precursor;
(3) Sintering, so that the first slurry is converted into a first filter layer, and the second slurry is converted into a second filter layer, thus obtaining a third precursor;
(4) Loading a nonmetallic oxide film anticorrosive layer on the outer surface and/or pore surface of the third precursor to obtain the composite porous film;
viscosity: the first slurry > the second slurry.
The first filter layer and the second filter layer are connected into a whole, so that the strength of the porous film can be obviously improved; when the first filter layer is combined with the support body, the second filter layer is arranged, so that the apparent mass of the second filter layer can be improved; the first anti-corrosion layer and the second anti-corrosion layer can protect the whole porous film, so that the phenomenon of local corrosion (acid condensation) can be prevented when certain low-temperature working conditions are in service, and the service life is further prolonged. When the first anti-corrosion layer and the second anti-corrosion layer are provided at the same time, the first anti-corrosion layer and the second anti-corrosion layer cooperate, so that the whole porous film can be fully protected; when the viscosity of the second slurry is smaller than that of the first slurry, the pore diameter of the porous film is changed in a gradient manner, and the binding force between the first filter layer and the support body is stronger. SiO (SiO) 2 The film has the advantages of easy acquisition, toughness, wear resistance, high corrosion resistance and the like.
Further, pore size: the first filter structure is greater than the second filter structure.
Further, the viscosity of the first slurry is 5000-15000 mPa.s; the viscosity of the second slurry is 40-80 mPas.
Further, in the step (1), the first slurry is attached to the support body by adopting a doctor blade coating mode; and (2) attaching the second slurry to one side of the first precursor in a spraying mode.
Further, the first slurry and the second slurry adopt the same raw material powder.
Further, the first slurry employs a multi-component binder; the second slurry employs a one-component binder.
Further, the binder is selected from CMC (sodium carboxymethyl cellulose), SBR (styrene butadiene rubber) and PVA (polyvinyl alcohol).
Further, the non-metal oxideThe film is SiO 2 A film; the SiO is 2 The thickness of the film is 10-20 mu m.
Further, the SiO 2 The film is composed of SiO attached to the outer surface of the third precursor and/or the pore surface 2 And sintering the sol to obtain the final product.
In order to achieve the above object, the fourth preparation method of the composite porous film provided by the present invention comprises the following steps:
(1) Preparing a first slurry with the viscosity of 5000-15000 mPa.s by taking alloy powder as raw material powder and CMC and SBR as binders, and then enabling a support body carrying the first slurry to pass through a gap between two scrapers at the speed of 3-5 m/min to obtain a first precursor;
(2) Preparing second slurry with the viscosity of 40-80 mPas by taking alloy powder as raw material powder and PVA as a binder, spraying the second slurry on one side of the first precursor, and drying to obtain a second precursor;
(3) Rolling the second precursor;
(4) Sintering the rolled second precursor: the first stage is heat-preserving for 60-90 min at 120-250 ℃, the second stage is heat-preserving for 60-120 min at 500-600 ℃, and the third stage is heat-preserving for 90-180 min at 900-1150 ℃ to obtain a third precursor;
(5) Soaking the third precursor in SiO 2 And (3) taking out the sol, and sintering at 500-600 ℃, namely forming a first anti-corrosion layer on the pore surface of the third precursor and forming a second anti-corrosion layer on the outer surface of the third precursor, thereby obtaining the composite porous film.
In order to achieve the above object, the fifth preparation method of the composite porous film provided by the present invention includes the following steps:
(1) Obtaining first slurry, and then attaching the first slurry to the support body, so that the pores of the support body are partially or completely filled with the first slurry, and a first precursor is obtained;
(2) Obtaining second slurry, attaching the second slurry to one side of the first precursor, and drying to obtain a second precursor;
(3) Sintering, so that the first slurry is converted into a first filter layer, and the second slurry is converted into a second filter layer, thus obtaining a third precursor;
(4) Loading an alloy film anticorrosive layer on the outer surface and/or pore surface of the third precursor to obtain the composite porous film;
the first slurry and the second slurry adopt the same raw material powder.
The first filter layer and the second filter layer are connected into a whole, so that the strength of the porous film can be obviously improved; when the first filter layer is combined with the support body, the second filter layer is arranged, so that the apparent mass of the second filter layer can be improved; the first anti-corrosion layer and the second anti-corrosion layer can protect the whole porous film, so that the phenomenon of local corrosion (acid condensation) can be prevented when certain low-temperature working conditions are in service, and the service life is further prolonged. When the first anti-corrosion layer and the second anti-corrosion layer are provided at the same time, the first anti-corrosion layer and the second anti-corrosion layer cooperate, so that the whole porous film can be fully protected; when the first slurry and the second slurry adopt the same raw material powder, the binding force between the first filter layer and the second filter layer can be improved.
Further, pore size: the first filter structure is greater than the second filter structure.
Further, viscosity: the first slurry > the second slurry.
Further, the viscosity of the first slurry is 5000-15000 mPa.s; the viscosity of the second slurry is 40-80 mPas.
Further, in the step (1), the first slurry is attached to the support body by adopting a doctor blade coating mode; and (2) attaching the second slurry to one side of the first precursor in a spraying mode.
Further, the first slurry employs a multi-component binder; the second slurry employs a one-component binder.
Further, the binder is selected from CMC, SBR and PVA.
Further, the alloy film is formed by converting an alloy catalytic liquid attached to the outer surface and/or the pore surface of the third precursor; the alloy film and the raw material powder contain the same metal element. The thickness of the mode of converting the alloy catalytic liquid into the alloy film is controllable, and the cost is low; when the alloy film and the raw material powder contain the same metal element, the binding force between the third precursor and the alloy film is stronger.
Further, the alloy film is a Ni-P alloy film; the thickness of the alloy film is 10-20 mu m. The Ni-P alloy coating has fine and compact structure and high bonding strength with the filter layer, can achieve the purposes of no peeling, no falling and no rust at 350-400 MPa, and has excellent corrosion resistance and wear resistance.
In order to achieve the above object, the sixth preparation method of the composite porous film provided by the present invention includes the following steps:
(1) Preparing a first slurry with the viscosity of 5000-15000 mPa.s by taking nickel alloy powder as raw material powder and CMC and SBR as binders, and then enabling a support body carrying the first slurry to pass through a gap between two scrapers at the speed of 3-5 m/min to obtain a first precursor;
(2) Preparing a second slurry with the viscosity of 40-80 mPa.s by taking nickel alloy powder as raw material powder and PVA as a binder, spraying the second slurry on one side of the first precursor, and drying to obtain a second precursor;
(3) Rolling the second precursor;
(4) Sintering the rolled second precursor: the first stage is heat-preserving for 60-90 min at 120-250 ℃, the second stage is heat-preserving for 60-120 min at 500-600 ℃, and the third stage is heat-preserving for 90-180 min at 900-1150 ℃ to obtain a third precursor;
(5) Preparing Ni-P alloy catalytic liquid: comprises a solvent, nickel salt, hypophosphite, a buffering agent, a complexing agent, ammonia potassium powder, sulfur gloss powder, sodium iodide powder and a wetting agent; soaking the third precursor in the catalytic liquid, taking out, and baking at 100-140 ℃ to convert the catalytic liquid into the Ni-P alloy film, namely forming a first anti-corrosion layer on the pore surfaces of the third precursor and forming a second anti-corrosion layer on the outer surfaces of the pores of the third precursor, thus obtaining the composite porous film.
The invention is further described below with reference to the drawings 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 form a part hereof, are shown by way of illustration and not of limitation, and in which are shown by way of illustration and description of the invention. In the drawings:
FIG. 1 is a schematic structural view of a composite porous film according to examples 1 to 3 of the present invention.
FIG. 2 is an enlarged view of a portion of the composite porous film of examples 1-3 of the present invention.
1-a support, 21-a first filter layer, 22-a second filter layer, 31-a first corrosion protection layer, 32-a second corrosion protection layer.
Detailed Description
The present invention will now be described more fully hereinafter with reference to the accompanying drawings. Those of ordinary skill in the art will be able to implement the invention based on these descriptions. Before describing the present invention with reference to the accompanying drawings, it should be noted in particular that:
the technical solutions and technical features provided in the sections including the following description in the present invention may be combined with each other without conflict.
In addition, the embodiments of the present invention referred to in the following description are typically only some, but not all, embodiments of the present invention. Therefore, all other embodiments, which can be made by one of ordinary skill in the art without undue burden, are intended to be within the scope of the present invention, based on the embodiments of the present invention.
Terms and units in relation to the present invention. The terms "comprising," "having," and any variations thereof in the description and claims of the invention and in the relevant sections are intended to cover a non-exclusive inclusion.
Example 1
The composite porous membrane shown in fig. 1-2 comprises a first filter structure, a second filter structure and a corrosion protection layer; the first filtering structure comprises a supporting body 1 and a first filtering layer 21, wherein the pores of the supporting body 1 are fully filled by the first filtering layer 21, and the first filtering layer 21 is symmetrically distributed in the thickness direction of the supporting body 1; the second filter structure includes a second filter layer 22 on one side of the first filter structure; the thickness of the second filter layer 22 is 0.05mm.
The anti-corrosion layers comprise a first anti-corrosion layer 31 arranged on the pore surfaces of the first filtering structure and the second filtering structure, a second anti-corrosion layer 32 arranged on the outer surfaces of the first filtering structure and the second filtering structure, and a third anti-corrosion layer arranged between the supporting body 1 and the first filtering layer 21.
The first and second anticorrosive layers 31 and 32 are metal oxide films, which are Al 2 O 3 A film. The third anti-corrosion layer is a metal plating layer arranged on the surface of the support body 1; the metal coating is a nickel layer.
The thickness of the first anticorrosive layer 31 is 10-20 μm; the thickness of the second anticorrosive layer 32 is 10 to 20 μm.
The aperture of the first filtering structure is 30-50 mu m, the aperture of the second filtering structure is 15-25 mu m, and the aperture is as follows: the first filter structure is greater than the second filter structure.
The support body 1 is a metal screen mesh with the thickness of 0.05mm and made of 50 meshes and 316L materials.
The preparation method of the composite porous film comprises the following steps:
(1) Preparing a first slurry with the viscosity of 5000 mPa.s by taking stainless steel powder as raw material powder and CMC and SBR as binders, and then enabling a support body 1 carrying the first slurry to pass through a space between two scrapers at the speed of 4m/min to obtain a first precursor;
(2) Preparing second slurry with the viscosity of 40 mPa.s by taking stainless steel powder as raw material powder and PVA as a binder, spraying the second slurry on one side of the first precursor, and drying to obtain a second precursor;
(3) Rolling the second precursor;
(4) Sintering the rolled second precursor: the first stage is kept at 200 ℃ for 80min, the second stage is kept at 500 ℃ for 120min, and the third stage is kept at 1150 ℃ for 90min, so as to obtain a third precursor;
(5) Soaking the third precursor in Al sol, taking out, sintering at 550 deg.C to convert Al sol into Al 2 O 3 And forming a first anticorrosive layer 31 on the pore surfaces of the third precursor and forming a second anticorrosive layer 32 on the outer surface of the third precursor to obtain the composite porous film.
Example 2
The composite porous membrane shown in fig. 1-2 comprises a first filter structure, a second filter structure and a corrosion protection layer; the first filtering structure comprises a supporting body 1 and a first filtering layer 21, wherein the pores of the supporting body 1 are fully filled by the first filtering layer 21, and the first filtering layer 21 is symmetrically distributed in the thickness direction of the supporting body 1; the second filter structure includes a second filter layer 22 on one side of the first filter structure; the thickness of the second filter layer 22 is 0.1mm.
The anti-corrosion layers comprise a first anti-corrosion layer 31 arranged on the pore surfaces of the first filtering structure and the second filtering structure, a second anti-corrosion layer 32 arranged on the outer surfaces of the first filtering structure and the second filtering structure, and a third anti-corrosion layer arranged between the supporting body 1 and the first filtering layer 21.
The first and second anticorrosive layers 31 and 32 are non-metal oxide films, and the metal oxide films are SiO 2 A film. The third anti-corrosion layer is a metal plating layer arranged on the surface of the support body 1, and the metal plating layer is a zinc layer.
The thickness of the first anticorrosive layer 31 is 10-20 μm; the thickness of the second anticorrosive layer 32 is 10 to 20 μm.
The aperture of the first filtering structure is 30-50 mu m, the aperture of the second filtering structure is 15-25 mu m, and the aperture is as follows: the first filter structure is greater than the second filter structure.
The support body 1 is a metal screen mesh with the thickness of 0.2mm and made of 50 meshes and 316L materials.
The preparation method of the composite porous film comprises the following steps:
(1) Preparing a first slurry with viscosity of 15000 mPa.s by taking Ha-type alloy powder as raw material powder and CMC and SBR as binders, and then enabling a support body 1 carrying the first slurry to pass through a space between two scrapers at a speed of 4m/min to obtain a first precursor;
(2) Preparing second slurry with viscosity of 60 mPa.s by taking Ha alloy powder as raw material powder and PVA as a binder, spraying the second slurry on one side of the first precursor, and drying to obtain a second precursor;
(3) Rolling the second precursor;
(4) Sintering the rolled second precursor: the first stage is kept at 200 ℃ for 80min, the second stage is kept at 550 ℃ for 90min, and the third stage is kept at 1000 ℃ for 130min, so as to obtain a third precursor;
(5) Soaking the third precursor in SiO 2 Soaking in the sol for 10min, taking out, drying, and sintering at 550 ℃ for 1h to form a first anti-corrosion layer 31 on the pore surface of the third precursor and a second anti-corrosion layer 32 on the outer surface of the third precursor, thus obtaining the composite porous film.
Example 3
The composite porous membrane shown in fig. 1-2 comprises a first filter structure, a second filter structure and a corrosion protection layer; the first filtering structure comprises a supporting body 1 and a first filtering layer 21, wherein the pores of the supporting body 1 are fully filled by the first filtering layer 21, and the first filtering layer 21 is symmetrically distributed in the thickness direction of the supporting body 1; the second filter structure includes a second filter layer 22 on one side of the first filter structure; the thickness of the second filter layer 22 is 0.15mm.
The anti-corrosion layers comprise a first anti-corrosion layer 31 arranged on the pore surfaces of the first filtering structure and the second filtering structure, a second anti-corrosion layer 32 arranged on the outer surfaces of the first filtering structure and the second filtering structure, and a third anti-corrosion layer arranged between the supporting body 1 and the first filtering layer 21.
The first anticorrosive layer 31 and the second anticorrosive layer 32 are alloy films, and the alloy films are Ni-P alloy films; the third anti-corrosion layer is a metal plating layer arranged on the surface of the support body 1, and the metal plating layer is a chromium layer.
The thickness of the first anticorrosive layer 31 is 10-20 μm; the thickness of the second anticorrosive layer 32 is 10 to 20 μm.
The aperture of the first filtering structure is 30-50 mu m, the aperture of the second filtering structure is 15-25 mu m, and the aperture is as follows: the first filter structure is greater than the second filter structure.
The support body 1 is a metal screen mesh with the thickness of 0.6mm and made of 50 meshes and 316L materials.
The preparation method of the composite porous film comprises the following steps:
(1) Preparing a first slurry with viscosity of 10000 mPa.s by taking nickel alloy powder as raw material powder and CMC and SBR as binders, and then enabling a support body 1 carrying the first slurry to pass through a space between two scrapers at a speed of 4m/min to obtain a first precursor;
(2) Preparing a second slurry with the viscosity of 80 mPa.s by taking nickel alloy powder as raw material powder and PVA as a binder, spraying the second slurry on one side of the first precursor, and drying to obtain a second precursor;
(3) Rolling the second precursor;
(4) Sintering the rolled second precursor: the first stage is kept at 200 ℃ for 80min, the second stage is kept at 600 ℃ for 60min, and the third stage is kept at 900 ℃ for 180min, so as to obtain a third precursor;
(5) Preparing Ni-P alloy catalytic liquid: comprises a solvent, nickel salt, hypophosphite, a buffering agent, a complexing agent, ammonia potassium powder, sulfur gloss powder, sodium iodide powder and a wetting agent; soaking the third precursor in a catalytic liquid, taking out the catalytic liquid after soaking for 25min at 80-85 ℃, and then baking for 4h at 120 ℃ to convert the catalytic liquid into a Ni-P alloy film, namely forming a first anti-corrosion layer 31 on the pore surface of the third precursor and forming a second anti-corrosion layer 32 on the outer surface of the pore surface of the third precursor, thus obtaining the composite porous film.
The Al sol can be prepared by the following preparation method:
by pseudo-boehmite (AlOOH.nH) 2 O) is used as a raw material, pseudo-boehmite is weighed according to the concentration of 10% -30%, and is added into deionized water, the temperature is controlled to be 30-50 ℃, nitric acid solution is slowly dripped in a stirring state, the concentration of the nitric acid solution is 5%, the pH value of the final solution is controlled to be 5-8, and the stirring time is 0.5-1 h, so that the Al sol is formed. In example 5, the concentration of the aqueous solution of pseudo-boehmite was 20%, the temperature was controlled at 40 °, the final pH was 6, and stirring was carried out for 1h; soaking the third precursor in Al sol in a vacuumizing mode to fill all pores of the third precursor with the Al sol, and then sintering at 500 ℃ for 1h after drying to form Al 2 O 3 A film.
SiO as described above 2 The sol may be prepared by, but is not limited to, the following methods:
volume ratio: ethyl orthosilicate: absolute ethyl alcohol: deionized water: concentrated sulfuric acid=15:45:5:0.07, absolute ethanol is divided into two parts, one part is uniformly mixed with tetraethoxysilane to form a solution a, and the other part is uniformly mixed with concentrated hydrochloric acid and deionized water to form a solution B. Slowly dripping the solution A into the solution B while continuously stirring the solution B, sealing after dripping, and continuously stirring for 3 hours; standing for 3 days to obtain SiO 2 And (3) sol.
The Ni-P alloy catalytic liquid can be prepared by the following formula:
the formula comprises water, nickel salt, sodium hypophosphite, buffering agent, complexing agent, ammonia potassium powder, sulfur light powder, sodium iodide powder and wetting agent. The component contents (weight ratio) in example 7: 90% of water, 2.8% of nickel sulfate, 2.6% of sodium hypophosphite, 1.4% of buffer, 3.0% of complexing agent, 0.14% of ammonia potassium powder, 0.002% of sulfur light powder, 0.008% of sodium iodide powder and 0.05% of wetting agent, wherein the complexing agent is citrate or sodium hexametaphosphate, and the buffer is a mixed solution of weak acid and salt thereof (such as HAc and NaAc) or a mixed solution of weak base and salt thereof (such as NH) 3 ·H 2 O and NH 4 Cl), and the wetting agent is silanol nonionic surfactant.
85% of the technical raw materials of the alloy catalytic liquid adopt food-grade additives, accord with the ROSH standard, have no toxicity and three wastes, do not harm human bodies and do not pollute the environment.
In order to reduce the moving resistance of the support 1 between the two blades on the premise that the first slurry sufficiently fills the pores of the support 1, the distance between the two blades may be made larger than the thickness of the support 1, and thus, the first filter layer 21 is provided on both the pore surface and the outer surface of the support 1. For a flexible film (composite porous film with a total thickness > 200 μm), the thickness of the first filter layer 21 on the outer surface of the support 1 is preferably 0.035 to 0.05mm; for a paper type film (composite porous film having a total thickness of 200 μm or less), the thickness of the first filter layer 21 on the outer surface of the support 1 is preferably 0.005 to 0.015mm. If it is desired to form a thicker first filter layer 21 on the outer surface of the support 1, the doctor blade pitch can be further increased.
The bulk density of the powder can be improved by rolling, and the aperture is reduced. The thickness of the porous film can be further controlled by controlling the rolling gap.
In examples 5 to 7, in order to promote the reaction liquid (Al sol, siO 2 Sol and alloy catalytic liquid) enters the pores of the third precursor, the flow of the reaction liquid is promoted by adopting a vacuumizing mode, and the vacuum degree is 0.1-1 kPa.
The content of the present invention is described above. Those of ordinary skill in the art will be able to implement the invention based on these descriptions. Based on the foregoing, all other embodiments that may be obtained by one of ordinary skill in the art without undue burden are within the scope of the present invention.
Claims (8)
1. The preparation method of the composite porous film comprises the following steps:
(1) Obtaining first slurry, and then attaching the first slurry to a support body, so that the pores of the support body are partially or completely filled with the first slurry, and a first precursor is obtained;
(2) Obtaining second slurry, attaching the second slurry to one side of the first precursor, and drying to obtain a second precursor;
(3) Sintering, so that the first slurry is converted into a first filter layer (21), and the second slurry is converted into a second filter layer (22), thus obtaining a third precursor;
(4) Loading an alloy film anticorrosive layer on the outer surface and/or pore surface of the third precursor to obtain the composite porous film;
the first slurry and the second slurry adopt the same raw material powder; viscosity: the first slurry is greater than the second slurry;
pore diameter: the first filter structure > the second filter structure, the first filter structure comprises a support body and a first filter layer, and the second filter structure comprises a second filter layer.
2. The method for preparing a composite porous film according to claim 1, wherein: the viscosity of the first slurry is 5000-15000 mPa.s; the viscosity of the second slurry is 40-80 mPas.
3. The method for preparing a composite porous film according to claim 2, wherein: the first sizing agent is attached to the supporting body in a doctor blade coating mode; and (2) attaching the second slurry to one side of the first precursor in a spraying mode.
4. The method for preparing a composite porous film according to claim 1, wherein: the first sizing agent adopts a multi-component binder; the second slurry employs a one-component binder.
5. The method for preparing a composite porous film according to claim 4, wherein: the binder is selected from CMC, SBR and PVA.
6. The method for preparing a composite porous film according to claim 1, wherein: the alloy film is formed by converting alloy catalytic liquid attached to the outer surface and/or the pore surface of the third precursor; the alloy film and the raw material powder contain the same metal element.
7. The method for preparing a composite porous film according to claim 6, wherein: the alloy film is a Ni-P alloy film; the thickness of the Ni-P alloy film is 10-20 mu m.
8. The preparation method of the composite porous film comprises the following steps:
(1) Preparing a first slurry with the viscosity of 5000-15000 mPa.s by taking nickel alloy powder as raw material powder and CMC and SBR as binders, and then enabling a support body carrying the first slurry to pass through a gap between two scrapers at the speed of 3-5 m/min to obtain a first precursor;
(2) Preparing a second slurry with the viscosity of 40-80 mPa.s by taking nickel alloy powder as raw material powder and PVA as a binder, spraying the second slurry on one side of the first precursor, and drying to obtain a second precursor;
(3) Rolling the second precursor;
(4) Sintering the rolled second precursor: the first stage is heat-preserving for 60-90 min at 120-250 ℃, the second stage is heat-preserving for 60-120 min at 500-600 ℃, and the third stage is heat-preserving for 90-180 min at 900-1150 ℃ to obtain a third precursor;
(5) Preparing Ni-P alloy catalytic liquid: comprises a solvent, nickel salt, hypophosphite, a buffering agent, a complexing agent, ammonia potassium powder, sulfur gloss powder, sodium iodide powder and a wetting agent; soaking the third precursor in the catalytic liquid, taking out, and baking at 100-140 ℃ to convert the catalytic liquid into the Ni-P alloy film, namely forming a first anticorrosive layer (31) on the pore surfaces of the third precursor and forming a second anticorrosive layer (32) on the outer surfaces of the pores of the third precursor, thus obtaining the composite porous film.
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