CN110613983A - Method for manufacturing filter assembly - Google Patents
Method for manufacturing filter assembly Download PDFInfo
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- CN110613983A CN110613983A CN201810631365.2A CN201810631365A CN110613983A CN 110613983 A CN110613983 A CN 110613983A CN 201810631365 A CN201810631365 A CN 201810631365A CN 110613983 A CN110613983 A CN 110613983A
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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
- B01D46/0001—Making filtering elements
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C09D127/18—Homopolymers or copolymers of tetrafluoroethene
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/002—Priming paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2/00—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon
- C10G2/30—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen
- C10G2/32—Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts
- C10G2/34—Apparatus, reactors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention relates to the field of filter assemblies, and discloses a preparation method of a filter assembly, which comprises a porous matrix with micron pore channels and a non-stick coating positioned in the pore channels; the preparation method comprises the following steps: loading a non-stick coating on the porous substrate, performing ultrasonic treatment, and introducing airflow to allow the non-stick coating to enter the pore canal, wherein the ultrasonic treatment has an ultrasonic frequency of 20-80kHz and a sound intensity of 0.2-2W/cm2. The prepared filter assembly is used as a filter arranged in a Fischer-Tropsch synthesis reactor, so that the risk of agglomeration and blockage of catalyst particles on the surface of the filter is reduced, and the time is increasedFlux and reactor operating life, while improving filtration efficiency.
Description
Technical Field
The invention relates to the field of filter assemblies, in particular to a preparation method of a filter assembly.
Background
The capacity of the domestic Fischer-Tropsch synthesis device reaches 560 ten thousand tons per year, and the potential capacity reaches 2000 ten thousand tons per year. The existing slurry bed Fischer-Tropsch synthesis device mostly adopts a metal internal filter to separate the catalyst from the liquid wax. Because the catalyst is fine solid particles and is easy to break to generate fine powder in the flowing process, the filter is easy to block, emergency stop is forced, and the production cost is greatly increased. If the surface of the existing filter is coated into a non-sticky and self-lubricating surface through technical transformation, the risk of catalyst particles gathering on the inner and outer surfaces of the filter can be reduced, the filtering effect is improved, and the service life of the filter is prolonged.
CN1608174A, DE4239391C2 and CN101253004A all disclose coating methods of fluoropolymer on oxide ceramic layers formed of metals with thin barrier layers as boundary layers towards the metals, which are mainly to subject fluoropolymer particles in a suitable solvent to varying pressure conditions suitable for the impregnation system, to achieve fine branching of the fluoropolymer particles into the oxide ceramic layer by means of establishing and releasing a vacuum. The method is generally used for coating of non-permeable micropores and plays a role in improving the stability of surface chemistry, heat and electricity, but is not suitable for coating of filter components with permeable micropores such as metal powder sintering, ceramic powder sintering and the like.
CN1327964A discloses a surface coating process for an aluminum melt purification composite filter, which comprises the following steps: preheating the filter to 650-700 ℃, then immersing the filter into a molten universal flux (KCl: NaCl ═ 1: 1), standing for 5 minutes, taking out and naturally cooling, and removing redundant coating materials in the filter to obtain the inner surface coating of the filter with the thickness of 1-100 mu m for purifying the aluminum melt. The process can be used for dip-coating of large-aperture porous materials, but is not suitable for micro-scale aperture materials, and the uniformity of the coating cannot be ensured.
CN103205142A discloses an organic modified ceramic non-stick coating and a coating method, which solve the problems of poor adhesion and poor toughness of the existing ceramic non-stick coating, and the coating method adopts a common spraying method and is not suitable for coating porous materials such as woven sintering of a wire mesh, powder sintering and the like.
CN105727627A relates to a porous material and a preparation method thereof, wherein a thermoplastic resin coating and solid particles are loaded on the pore surfaces of a substrate by a spraying or dipping method to form a composite coating, the method significantly increases the specific surface area of the composite coating and forms secondary voids, and the porous material is mainly used for air purification. The pore diameter formed by the method after coating is not uniform, the pore diameter of the pore is not easy to control, and the coating is easy to fall off at high temperature.
In summary, in the existing filter element coating technologies, it is impossible to effectively coat the filter element with abundant irregular micro-scale pore channels, and therefore, there is a need to develop a new coating technology to improve the uniformity of coating inside the pore channels, so as to improve the service life or application field of the porous filter element.
Disclosure of Invention
The present invention is directed to overcoming the above problems of the prior art and to providing a novel method of making a filter assembly.
The invention provides a preparation method of a filter assembly, which comprises a porous matrix with micron pore channels and a non-stick coating positioned in the pore channels; the preparation method comprises the following steps: loading a non-stick coating on the porous substrate, performing ultrasonic treatment, and introducing airflow to allow the non-stick coating to enter the pore canal, wherein the ultrasonic treatment has an ultrasonic frequency of 20-80kHz and a sound intensity of 0.2-2W/cm2。
The invention carries out ultrasonic treatment on the porous matrix loaded with the non-stick coating under certain conditions, so that the non-stick coating generates an ultrasonic cavitation phenomenon, enters the inside of a larger pore passage of the porous matrix and also enters a smaller pore passage, and the blockage of the pore passage by the coating can be avoided by combining with the introduced air flow. The prepared filter assembly can ensure higher time flux. According to one embodiment, the filter assembly is used as a filter installed in a Fischer-Tropsch synthesis reactor, so that the risk of catalyst particles blocking on the surface of the filter is reduced, the time flux and the service life of the reactor are improved, and the filtering efficiency is improved.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a preparation method of a filter assembly, which comprises a porous matrix with micron pore channels and a non-stick coating positioned in the pore channels; the preparation method comprises the following steps: and loading a non-stick coating on the porous substrate, and then carrying out ultrasonic treatment to enable the non-stick coating to enter the inside of the pore channel.
According to the method, the ultrasonic frequency of the ultrasonic treatment is 20-80kHz, and the sound intensity is 0.2-2W/cm2This avoids the generation of a large amount of bubbles. Preferably, the ultrasonic frequency of the ultrasonic treatment is 30-60kHz, and the sound intensity is 0.3-0.7W/cm2。
It will be understood by those skilled in the art that the non-stick coating (often referred to as a polymer emulsion) generates ultrasonic cavitation during the ultrasonic treatment. Specifically, microbubbles in the emulsion vibrate under the action of a sound field to generate a plurality of small bubbles with different sizes, part of the bubbles grow rapidly in a negative pressure period and are closed suddenly in a positive pressure period, a micro shock wave with the pressure of hundreds to thousands of Pa is generated during closing, and thousands of atmospheric pressures are generated around the bubbles due to violent collision. In addition, the ultrasonic cavitation phenomenon is accompanied by the generation of various physical effects, including mechanical effects (shock waves, micro-jets), thermal effects (local high temperature, overall temperature rise), optical effects, activation effects, and the like. Through the action of ultrasonic wave, coating emulsion generates shock wave and micro-jet in the hole, so that the emulsion enters the pore canal of the porous base material in the repeated collision and vibration processes, and simultaneously, emulsion particles collide with each other in the ultrasonic process to induce the emulsion to be uniformly coated, namely the coating uniformity of the porous base material is ensured.
Within the above ranges, the specific ultrasonic frequency and ultrasonic sound intensity can be determined by one skilled in the art in view of the non-stick coating, as long as the stability of the coating itself is not compromised (e.g., does not break the emulsion).
According to the method of the present invention, the time of the ultrasonic treatment can be determined according to the viscosity of the non-stick coating and the like, and generally can be 10 to 60min, preferably 20 to 40 min.
According to the method of the present invention, in the ultrasonic treatment, the ultrasonic wave is preferably longitudinal wave, which is more favorable for orientation and promotes the flow of the coating material into the pore canal. The loading mode of the ultrasonic waves can be continuous loading or intermittent loading, and is preferably intermittent loading, so that demulsification caused by local temperature change can be further avoided, and the uniform distribution of the coating in the pore channels is facilitated. The loading frequency of the intermittent loading can be 0.5-10Hz, preferably 1-5 Hz.
The invention is suitable for coating any porous matrix with micron-sized pore channels to prepare the filter component, and therefore, the type of the porous matrix is not particularly limited. For example, the porous matrix may be selected from a metal powder sintered filter element, a metal wire mesh woven filter element, a ceramic powder sintered filter element, an ultrafiltration membrane, or a hollow fiber membrane.
Preferably, the porous matrix is selected from a metal powder sintered filter element, a metal wire mesh woven filter element or a ceramic powder sintered filter element.
Further preferably, the porous matrix is selected from a metal powder sintered filter element or a metal wire mesh woven filter element, and the preparation method further comprises the following steps: and before loading, sequentially carrying out alkali washing and water washing on the surface of the porous matrix to remove oil stains and impurities on the metal surface. In addition, in order to improve the adhesion of the coating on the surface of the filter element, the metal surface can be subjected to sanding treatment.
In the invention, the metal powder sintered filter element, the metal wire mesh woven filter element or the ceramic powder sintered filter element can be a conventional choice of a filter in a Fischer-Tropsch synthesis slurry bed reactor, and the average pore diameter of the filter is generally 20-40 mu m.
It will be appreciated by those skilled in the art that the filter element to be coated comprises a filtrate tube, the cylindrical body of which is surrounded by a porous medium formed of a metal or ceramic material, one end of the filtrate tube and the part of the porous medium being sealed. The method of the supporting is not particularly limited in the present invention, and for example, the supporting may be selected from a dropping method and/or a dipping method. In particular, the non-stick coating can be dropped onto the porous substrate or the porous substrate can be dipped into the non-stick coating. When the dropping method is employed, it preferably includes the steps of: the coating (priming paint and finish paint) is absorbed by a dropper and is uniformly dripped on the surface of the filter element, after the coating permeates into the sample, the coating is dripped from the filtrate pipe, the coating flows downwards along the filtrate pipe into the filter element, and at the moment, the suction pipe or an ear washing ball is repeatedly blown and sucked into the filtrate pipe (namely, the coating is squeezed and pinched along the axial direction of the filtrate pipe), so that the coating inside and outside the filter element is communicated, and the coating is ensured to be full of the whole microporous channel of the filter element. In addition, for the non-stick paint with larger surface tension, a vacuum infiltration mode can be adopted to increase the contact area of the paint and the substrate, and the vacuum infiltration mode is well known in the art and is not repeated in the invention.
According to the method of the present invention, the time of the loading is preferably such that the porous matrix is saturated. The criteria for the saturation are: after the coating is applied to the porous substrate, surface percolation occurs after a period of time after the coating is absorbed by the substrate. In the present invention, saturation is typically achieved by dipping the porous substrate with the non-stick coating for more than 5 minutes.
According to the method, in order to ensure that the pore channels of the porous matrix are unblocked after ultrasonic treatment, the preparation comprises the following steps: and introducing airflow into the matrix after ultrasonic treatment. According to one embodiment, the gas flow is introduced into the porous substrate from the nozzle at one end (non-sealed end) of the filtrate tube, and the gas flow flows along the inside of the porous substrate to the outside through the porous medium under the action of pressure, so that the coated substrate is kept open. The speed of the air flow can be 0.1-0.5m/s, and the time of the air flow is 5-20 min.
The non-stick coating is not particularly limited in the present invention, and may be any of various conventional polymer emulsions used for coating the surface of existing filters, for example, a solution or emulsion of a fluorine-containing polymer capable of forming a fluorine-containing resin coating on the surface of a porous substrate. In addition, in order to dry the non-stick coating to form the non-stick coating and ensure the binding force between the coating and the substrate, after the non-stick coating is coated on the porous substrate (namely, after ultrasonic treatment and air flow introduction), the preparation method further comprises the following steps: sintering the porous substrate to form the non-stick coating. The sintering conditions are specifically determined according to the non-stick coating.
In order to further improve the adhesion of the coating to said porous substrate according to the method of the present invention, it is preferred that said non-stick coating comprises a primer and a top coat.
Preferably, the topcoat contains, based on the dry weight of the topcoat: 80-100 wt% of fluororesin, 0-10 wt% of pigment and filler and 0-10 wt% of nano silicon dioxide.
More preferably, the content of the fluororesin in the finish paint is 80-95 wt%, the content of the pigment and filler is 1-8 wt%, and the content of the nano-silica is 1-8 wt%, based on the dry weight of the finish paint.
Preferably, the primer contains, based on the dry weight of the primer: 40-80 wt% of fluororesin, 5-30 wt% of adhesive resin, 5-30 wt% of pigment and filler and 1-10 wt% of nano silicon dioxide.
More preferably, the primer contains 60-80 wt% of the fluororesin, 10-25 wt% of the binder resin, 5-20 wt% of the pigment and filler, and 5-10 wt% of the nano silica, based on the dry weight of the primer.
According to the method of the present invention, the binder resin can improve adhesion between the coating layer and the substrate. In order to further improve the high temperature resistance of the coating layer, the binder resin is preferably selected from one or more of polyether sulfone resin (PES), polyether ether ketone (PEEK), Polyamideimide (PAI), polyphenylene sulfide (PPS), polyether imide (PEI), and polyimide resin (PI).
More preferably, the binder resin is at least one selected from the group consisting of PAI, PEEK and PPS.
According to the method of the present invention, the fluororesin refers to a fluoropolymer, and may be a fluororesin commonly used in existing fluororesin coatings, and typically, in the top coat and the primer, the fluororesin may be the same or different, and may be respectively selected from one or more than two of Polytetrafluoroethylene (PTEF), perfluoroethylene propylene copolymer (FEP), tetrafluoroethylene-perfluoroalkylvinylether copolymer (PFA), ethylene-tetrafluoroethylene copolymer (ETFE), Polychlorotrifluoroethylene (PCTFE), ethylene-chlorotrifluoroethylene copolymer (ECTFE), polyvinylidene fluoride (PVDF), and polyvinyl fluoride (PVF).
Preferably, the fluororesin is selected from PTEF and/or PFA.
According to the method of the invention, the pigments and fillers provide the non-stick coating with high temperature and corrosion resistance, and are generally selected from inorganic substances having high temperature and corrosion resistance. In the top coat and the primer, the pigments and fillers can be the same or different, and are preferably selected from one or more of cobalt green, molybdenum disulfide, graphite, sericite and copper chrome black.
It will be understood by those skilled in the art that in the present invention, "dry weight" refers to the total weight of the remaining components of the primer, topcoat, which do not include solvent. In addition, the solvent content in the top coat and the primer can be 30-90 wt%, preferably 40-60 wt%, based on the total weight of the top coat and the primer, respectively.
According to the method of the present invention, the solvent preferably comprises water and an organic solvent, which may be selected according to the general class of resins in the components to dissolve or disperse the resin components to form an emulsion, and typically the organic solvent may be selected from organic amines and/or organic alcohols, wherein non-limiting examples of the organic amine include N-methylpyrrolidone, triethanolamine, and the like; non-limiting examples of the organic alcohol include propylene glycol, glycerin, furfuryl alcohol, and the like.
In the solvent, the mass ratio of water to the organic solvent may be 1: 0.05-1, preferably 1: 0.05-0.5.
In a preferred embodiment, the non-stick coating comprises the primer and the top coat, and accordingly the preparation method comprises the following two stages:
the first stage is as follows: loading the primer on the porous substrate, carrying out first ultrasonic treatment, introducing airflow to enable the primer to enter the pore canal, and carrying out first sintering to obtain the porous substrate coated with the primer;
and a second stage: and loading the finish paint on the porous substrate coated with the primer, carrying out second ultrasonic treatment, introducing airflow to enable the finish paint to enter the pore canal, and then carrying out second sintering.
In this embodiment, the ultrasonic treatment conditions and the gas flow-in conditions of the above two stages may be performed as described above. Preferably, the ultrasonic frequency of the first ultrasonic treatment and the ultrasonic frequency of the second ultrasonic treatment are respectively 30-60kHz, and the sound intensity is 0.3-0.7W/cm2The time is 20-40 min; the loading mode is intermittent loading, and more preferably, the frequency of the intermittent loading is 1-5 Hz. In addition, the above-mentioned operating conditions of the first ultrasonic treatment and the second ultrasonic treatment may be the same or different, and are preferably the same for convenience of operation.
Preferably, in the first stage and the second stage, the speed of the introduced gas flow is 0.1-0.3m/s respectively, and the introduction time is 5-10 min.
In this embodiment, the first sintering serves to dry the primer and chemically react the primer with the substrate surface, and the second sintering serves to dry the coating and react the primer and topcoat, thereby improving the adhesion of the overall non-stick coating to the substrate surface.
Specifically, the conditions of the first sintering include: the temperature is 100-190 ℃, preferably 150-180 ℃ and the time is 5-15 min. The conditions of the second sintering include: the temperature is 200-400 ℃, preferably 300-400 ℃, more preferably 350-390 ℃ and the time is 5-15 min.
In this embodiment, the first sintering and the second sintering may be performed in an oven, or may be performed under the condition of passing a heating gas flow. The purpose of the heated gas stream is to provide the required temperature for sintering and to allow sintering to proceed under ventilated conditions.
In addition, the invention aims to provide a method for improving the coating of non-stick paint in a porous matrix with microporous pore canals, so that the invention can also coat one or more layers of the same or different non-stick paints on the inner and outer surfaces of the matrix according to the specific application of the filter component, and adjust the paint concentration, the coating times, the ultrasonic frequency, the sound intensity, the time and the like to control the coating thickness and distribution according to the properties of the paints so as to improve the high temperature resistance, the wear resistance, the chemical corrosion resistance and the like of the porous component. When the prepared filter assembly is used for solid-liquid separation, the adhesion force of solid particles (such as metal catalyst particles) on the surface of a substrate can be reduced, the flow resistance of liquid on the surface of the substrate is reduced, the filtration flux is increased, and the separation efficiency between the solid particles and the liquid is improved. Meanwhile, the inner surface and the outer surface of the matrix have non-stick characteristics, so that the pore channels of the matrix are not easy to block, and even if the pore channels are occasionally blocked, the blockage can be easily removed by means of gas/liquid back flushing and the like, so that the service life of the matrix is prolonged. The filtering assembly obtained by the method can be widely applied to the fields of chemical separation, corrosion prevention, drag reduction, adhesion prevention, scaling prevention and the like.
According to a preferred embodiment, the porous matrix of the filter assembly is a woven wire mesh filter element, wherein the surface energy of the non-stick coating is less than or equal to 18.5mN/m and the static friction coefficient is less than or equal to 0.04. In addition, the filter assembly was thermally analyzed by DSC: the temperature is maintained at 260 ℃ and 270 ℃ for 48 hours, and the weight is not substantially lost; the filter assembly was maintained in hot oil at 260 ℃ and 270 ℃ for 8 hours without loss of weight, indicating that the filter assembly had excellent heat resistance. The filter assembly can be arranged in a low-temperature Fischer-Tropsch synthesis reactor for use, so that the risk of catalyst particles gathering on the inner surface and the outer surface of the filter is reduced, the filtering effect is improved, and the service life of the filter is prolonged.
The present invention will be described in detail below by way of examples.
In the following examples and comparative examples,
the wire mesh woven filter cores with different apertures are all made of stainless steel, and the specification is phi 20mm multiplied by 45 mm; the wall thickness of the filter element is 2 mm.
The ultrasonic generator was a KQ-300VDV, available from Kunshan ultrasonic instruments.
And (3) pore diameter testing: and testing the average pore size and the pore size distribution of the filter element before and after coating by using a pore size analyzer.
Surface energy testing: measured by DSA100 full-automatic contact angle measuring instrument according to the sitting drop method.
The method for testing the contact angle of water on the coating comprises the following steps: measured by DSA100 full-automatic contact angle measuring instrument according to the sitting drop method.
And (3) testing the friction coefficient: measured by a UMT-3 high-temperature friction abrasion tester (linear reciprocating type), the stroke is 3mm, the frequency is 1Hz, and Fz is-100 g.
And (3) time flux test: and (3) testing the water flux of the filter element before and after coating by using a liquid-liquid displacement method aperture analyzer, recording the flow Q flowing through the filter element in unit time under the condition of constant pressure difference (delta P is 0.01MPa), and dividing the cross section area A of the pore passage of the filter element by the Q to obtain the time flux.
The filter blockage test is implemented by specifically adopting an oil slurry cold mold filtration experiment: the clogging of the filter was measured on a slurry bed cold die test apparatus having a diameter of 150mm and a height of 2 m. Adopting a liquid wax system with 2.5 percent by weight of catalyst, and feeding air from the bottom of the reactor, wherein the air speed is 0.1-0.2 m/s; the filter element coated by the comparative example and the example is arranged at a position 1.2m away from the bottom of the reactor, liquid wax flows out of the filter by vacuum pumping negative pressure, and the catalyst forms a filter cake on the surface of the filter. The filter clogging was characterized by observing the filter cake and the filtration time.
The alkali liquor is 2 weight percent NaOH aqueous solution.
The fluoropolymer coating A is a primer, and the formula is as follows:
100 parts by weight of a solvent (consisting of water and N-methylpyrrolidone in a weight ratio of 1: 0.2);
70 parts of polytetrafluoroethylene, 10 parts of PFA, 6 parts of cobalt green, 12 parts of PAI resin and 2 parts of nano-silica.
The fluorine-containing polymer coating B is a finish coat, and the formula is as follows:
100 parts by weight of solvent (composed of water and triethanolamine in a weight ratio of 1: 0.1)
80 parts of polytetrafluoroethylene, 15 parts of PFA, 3 parts of molybdenum disulfide and 2 parts of nano silicon dioxide.
Example 1
Firstly, ultrasonically cleaning a metal wire mesh woven filter element in alkali liquor for 10min, then ultrasonically cleaning the metal wire mesh woven filter element by deionized water for 10min, and then drying the metal wire mesh woven filter element at 120 ℃.
Secondly, soaking the whole filter element in the fluoropolymer coating A in a cleaning tank of an ultrasonic generator, starting the generator to perform ultrasonic treatment after the filter element is saturated, wherein the ultrasonic frequency is 30kHz, and the ultrasonic sound intensity is 0.5W/cm2The ultrasonic time is 20min, the ultrasonic wave is longitudinal wave, the loading mode is intermittent loading, and the loading frequency is 1 Hz.
Thirdly, introducing air flow into the filter element, wherein the air flow speed is 0.1m/s, the introduction time is 8min, and then sintering the filter element at 180 ℃ for 10min to obtain the filter element coated with the primer;
fourthly, in a cleaning tank of an ultrasonic generator, dipping the filter element coated with the primer in the fluoropolymer coating B, after the filter element is saturated, starting the generator to carry out ultrasonic treatment, wherein the ultrasonic frequency is 30kHz, and the ultrasonic sound intensity is 0.5W/cm2The ultrasonic time is 20min, the ultrasonic wave is longitudinal wave, the loading mode is intermittent loading, and the loading frequency is 1 Hz.
And fifthly, introducing air flow into the filter element, wherein the air flow speed is 0.1m/s, the introduction time is 8min, and then sintering the filter element at 380 ℃ for 8min to obtain the coated filter element.
The properties of the filter element before and after coating are shown in table 1.
Example 2
Firstly, ultrasonically cleaning a metal wire mesh woven filter element in alkali liquor for 10min, then ultrasonically cleaning the metal wire mesh woven filter element by deionized water for 10min, and then drying the metal wire mesh woven filter element at 120 ℃.
Secondly, soaking the whole filter element in the fluoropolymer coating A in a cleaning tank of an ultrasonic generator, starting the generator to perform ultrasonic treatment after the filter element is saturated, wherein the ultrasonic frequency is 60kHz, and the ultrasonic sound intensity is 0.5W/cm2The ultrasonic time is 20min, the ultrasonic wave is longitudinal wave, the loading mode is intermittent loading, and the loading frequency is 1 Hz.
Thirdly, introducing air flow into the filter element, wherein the air flow speed is 0.2m/s, the introduction time is 5min, and then sintering the filter element at 180 ℃ for 10min to obtain the filter element coated with the primer;
fourthly, in a cleaning tank of an ultrasonic generator, dipping the filter element coated with the primer in the fluoropolymer coating B, after the filter element is saturated, starting the generator to carry out ultrasonic treatment, wherein the ultrasonic frequency is 60kHz, and the ultrasonic sound intensity is 0.5W/cm2The ultrasonic time is 20min, the ultrasonic wave is longitudinal wave, the loading mode is intermittent loading, and the loading frequency is 1 Hz.
And fifthly, introducing air flow into the filter element for 5min at the air flow speed of 0.2m/s, and sintering the filter element at 380 ℃ for 8min to obtain the coated filter element.
The properties of the filter element before and after coating are shown in table 1.
Example 3
Firstly, ultrasonically cleaning a metal wire mesh woven filter element in alkali liquor for 10min, then ultrasonically cleaning the metal wire mesh woven filter element by deionized water for 10min, and then drying the metal wire mesh woven filter element at 120 ℃.
Secondly, soaking the whole filter element in the fluoropolymer coating A in a cleaning tank of an ultrasonic generator, starting the generator to perform ultrasonic treatment after the filter element is saturated, wherein the ultrasonic frequency is 40kHz, and the ultrasonic sound intensity is 1W/cm2The ultrasonic time is 30min, the ultrasonic wave is longitudinal wave, the loading mode is intermittent loading, and the loading frequency is 1 Hz.
Thirdly, introducing air flow into the filter element, wherein the air flow speed is 0.1m/s, the introduction time is 5min, and then sintering the filter element at 180 ℃ for 10min to obtain the filter element coated with the primer;
fourthly, in a cleaning tank of an ultrasonic generator, dipping the filter element coated with the primer in the fluoropolymer coating B, after the filter element is saturated, starting the generator to carry out ultrasonic treatment, wherein the ultrasonic frequency is 30kHz, and the ultrasonic sound intensity is 1W/cm2The ultrasonic time is 30min, the ultrasonic wave is longitudinal wave, the loading mode is intermittent loading, and the loading frequency is 1 Hz.
Fifthly, introducing air flow into the filter element, wherein the air flow speed is 0.1m/s, the introduction time is 5min, and then sintering the filter element at 380 ℃ for 10min to obtain the filter element coated with the primer;
the properties of the filter element before and after coating are shown in table 1.
Example 4
A wire mesh woven filter element was coated in the same manner as in example 1 except that the frequency of intermittent loading was controlled to 10Hz in the second step and the fourth step, respectively, to obtain a coated filter element, the properties of which before and after coating were as shown in table 1.
Example 5
A wire mesh woven filter element was coated in the same manner as in example 1, except that in the second step and the fourth step, the ultrasonic frequency was controlled to 80kHz and the ultrasonic sound intensity was controlled to 1.5W/cm, respectively2To give a coated filter element having the properties before and after coating as shown in table 1.
Comparative example 1
Ultrasonically cleaning the metal wire mesh woven filter element in alkali liquor for 10min, then ultrasonically cleaning the metal wire mesh woven filter element by deionized water for 10min, and then drying the metal wire mesh woven filter element at 120 ℃. The properties of the treated filter element are shown in table 1.
Comparative example 2
Firstly, ultrasonically cleaning a metal wire mesh woven filter element in alkali liquor for 10min, then ultrasonically cleaning the metal wire mesh woven filter element by deionized water for 10min, and then drying the metal wire mesh woven filter element at 120 ℃.
And secondly, soaking the whole filter element in the fluorine-containing polymer emulsion A, transferring the filter element to an oven after the filter element is saturated, and sintering the filter element for 10min at 180 ℃ to obtain the filter element coated with the primer.
And thirdly, dipping the filter element coated with the primer in the fluoropolymer coating B, transferring the filter element to a baking oven after the filter element is saturated, and sintering the filter element for 8min at 390 ℃ to obtain the filter element with the coating.
The properties of the filter element before and after coating are shown in table 1.
TABLE 1
*: "front" means "the filter element before coating", "rear" means the filter element after coating, and in addition, other parameters of the examples which do not mention "front" and "rear" mean the performance after coating.
1: the filter cake distribution results are a comparison of the examples and comparative examples.
2: the cake thickness results compare the examples to the comparative examples.
As can be seen from Table 1, comparing examples 1-4 with comparative example 1, the filters of examples 1-4 have higher time flux and can improve the duration of single filtration, obviously reduce the blockage of the filter by catalyst particles in Fischer-Tropsch synthesis, reduce the liquid flow resistance and form thin and uniform filter cakes after filtration under the condition of equivalent pore size; in addition, the filter of example 5 has a smaller pore size, but its single filtration duration is also increased and its service life is longer than that of comparative example 1.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method of making a filter assembly comprising a porous substrate having micron channels and a non-stick coating within the channels; it is characterized in thatThe preparation method comprises the following steps: loading a non-stick coating on the porous substrate, performing ultrasonic treatment, and introducing airflow to allow the non-stick coating to enter the pore canal, wherein the ultrasonic treatment has an ultrasonic frequency of 20-80kHz and a sound intensity of 0.2-2W/cm2。
2. The method of claim 1, wherein the porous substrate is selected from a metal powder sintered filter element, a wire mesh woven filter element, or a ceramic powder sintered filter element.
3. The method of claim 2, wherein the porous substrate is selected from a metal powder sintered filter element or a metal wire mesh woven filter element, the method further comprising: and before carrying out loading, sequentially carrying out alkali washing and water washing on the surface of the porous matrix.
4. The method of any of claims 1-3, wherein the non-stick coating comprises a primer and a topcoat.
5. The production method according to claim 4, wherein the primer contains, based on the dry weight of the primer: 40-80 wt% of fluororesin, 5-30 wt% of adhesive resin, 5-30 wt% of pigment and filler and 0-10 wt% of nano silicon dioxide.
6. The method of claim 4, wherein the topcoat comprises, based on the dry weight of the topcoat: 80-100 wt% of fluororesin, 0-10 wt% of pigment and filler and 0-10 wt% of nano silicon dioxide.
7. The production method according to any one of claims 4 to 6, wherein the production method comprises the following two stages:
the first stage is as follows: loading the primer on the porous substrate, carrying out first ultrasonic treatment, introducing airflow to enable the primer to enter the pore canal, and carrying out first sintering to obtain the porous substrate coated with the primer;
and a second stage: and loading the finish paint on the porous substrate coated with the primer, carrying out second ultrasonic treatment, introducing airflow to enable the finish paint to enter the pore canal, and then carrying out second sintering.
8. The preparation method according to claim 7, wherein the ultrasonic frequencies of the first ultrasonic treatment and the second ultrasonic treatment are respectively 30-60kHz, and the sound intensity is 0.3-0.7W/cm2The time is 20-40min, and the loading mode is intermittent loading; preferably, the frequency of intermittent loading is 1-5 Hz.
9. The method according to claim 7, wherein the gas flow velocity in the first stage and the second stage is 0.1-0.3m/s and the time of the gas flow is 5-10 min.
10. The production method according to claim 7, wherein the conditions of the first sintering include: the temperature is 150 ℃ and 180 ℃, and the time is 5-15 min; and/or
The conditions of the second sintering include: the temperature is 300 ℃ and 400 ℃, and the time is 5-15 min.
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