CN103193513A - Coating method of silicon carbide ceramic membrane for high-temperature filtration - Google Patents
Coating method of silicon carbide ceramic membrane for high-temperature filtration Download PDFInfo
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- CN103193513A CN103193513A CN2013101302930A CN201310130293A CN103193513A CN 103193513 A CN103193513 A CN 103193513A CN 2013101302930 A CN2013101302930 A CN 2013101302930A CN 201310130293 A CN201310130293 A CN 201310130293A CN 103193513 A CN103193513 A CN 103193513A
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Abstract
The invention discloses a coating method of a silicon carbide ceramic membrane for high-temperature filtration. The method comprises the following steps: preparing an inorganic silicon carbide membrane slurry material which is stable, good in dispersibility and excellent in membrane-forming property by utilizing one or multiple solvents of glycerol, propylene glycol, ethanol, ethylene glycol and triethylene glycol; coating the filtering membrane by utilizing the air spraying technology; and performing heat treatment, thereby preparing the silicon carbide ceramic membrane which is uniform and integrated, controllable in thickness and large in size. Based on the reasonable design of a ceramic bonding agent for the filtering membrane, the chemical stability and the bonding strength of the filtering membrane are improved. The prepared silicon carbide ceramic membrane is simple in preparation process and easy in membrane-forming condition control, realizes reduction in cost and is convenient for industrialized production. The composite filtering material obtained by sintering at high temperature is suitable for the filtration purification of high-temperature fluids such as molten metal, high-temperature flue gas and the like.
Description
Technical field
The present invention relates to a kind of method for preparing the inorganic filter film, related to a kind of coating method that utilizes the aerial spraying technology to prepare complex silicon carbide porous ceramics filtering membrane more specifically, belonged to the porous ceramics field.
Background technology
The research of mineral membrane and application start from during the Second World War, and countries such as America and Europe utilize the uranium in the mineral membrane enrichment uranium ore.The nineties in last century, mineral membrane research enters with the gas delivery utilization to advocate peace mineral membrane separator---the stage of combination of reactors member, brings revolutionary variation to fields such as traditional chemical industry, petrochemical complex, biochemical industry, pharmaceutical industry, foodstuffs industry.
Mineral membrane has some incomparable advantages of traditional separatory membrane: Heat stability is good, chemical property be stable, clean convenience, long service life, regenerate easily, pore size distribution is narrow, and separation efficiency is high.Especially at high temperature, high pressure gas-solid separation field other filtering material incomparable advantage are arranged, it has become the core parts of high-temperature filter.Wherein asymmetric filtering material is the following direction in this field, and the paint-on technique of high uniformity both surface filtration film is one of gordian technique difficult problem of composite filter material.
The research of mineral membrane and industrialization key are the preparation of filtering membrane.The inorganic filter membrane preparation method mainly contains crystal pulling method, doctor-blade casting process, Film forming method, anodic oxidation, sol-gel method etc.The filtering membrane of crystal pulling method preparation is because gravitate, the even integrity of film is difficult to be guaranteed, doctor-blade casting process can only carry out plated film to the plate support body material of small size, thin film deposition and sol-gel method cost are too high, be difficult to realize industrial applications, anonizing is confined to metal oxide and carries out plated film.
Summary of the invention
The purpose of this invention is to provide a kind of high temperature filtration with the coating method of silicon carbide ceramics film, this method required equipment is simple, economical and practical, be easy to suitability for industrialized production, behind the supporter sintering, sprays the layer of fibers that one deck contains binding agent thereon.After the oven dry, recycling aerial spraying technology applies the evenly easy silicon carbide inorganic surfaces film of controlling of complete, thickness.
To achieve these goals, technical scheme of the present invention is: the coating method of high temperature filtration with the silicon carbide ceramics film is provided, comprise steps such as preparation carborundum porous ceramics supporter base substrate, preparation layer of fibers slurry, preparation uniform fiber layer slurry, the coating of uniform fiber layer slurry, filtering membrane pulp preparation and the coating of filtering membrane slurry, specific as follows:
(1) preparation carborundum porous ceramics supporter base substrate: be 10:0.5 ~ 3.3:0.5 ~ 4.0 by carborundum powder, vitrified bond, pore-forming material mass ratio, take by weighing the required amount of each raw material respectively, the preparation mass concentration is Xylo-Mucine (CMC) solution of 1.5wt%, the grain diameter of employed carborundum powder is 100 ~ 350 μ m, and it is that 65wt% potassium felspar sand, 12wt% burn kaolin and 23wt% quartz sand mixing and ball milling 20h configuration forms that vitrified bond consists of massfraction.Pore-forming material is graphite, and particle diameter is 10 ~ 60 μ m.Add carboxymethylcellulose sodium solution when stirring successively in beaker, after silicon carbide stirs, repeatedly add binding agent on a small quantity, carboxymethylcellulose sodium solution repeatedly adds pore-forming material on a small quantity.With dry-pressing formed after its mixing and stirring, pressure is 1 ~ 50MPa, and supporter thickness is 3 ~ 20mm, and diameter is 10 ~ 100mm; After will preparing the green compact drying, with temperature rise rate 2 ~ 30
oC/min presintering to 1000 ~ 1250 ℃, soaking time is 1 ~ 5h.Wherein the total mass of Xylo-Mucine (CMC) solution that adds several times is 5 ~ 20wt% of silicon carbide, binding agent, pore-forming material total mass;
(2) layer of fibers pulp preparation: the mullite fiber that takes by weighing, single diameter Distribution 0.5 ~ 15 μ m of aluminum silicate fiber, length-to-diameter ratio is greater than 10, the vitrified bond particle diameter is 1 ~ 40 μ m, and wherein the mass ratio of mullite fiber, aluminum silicate fiber, vitrified bond is 0.5 ~ 4:0.5 ~ 3.5:0.1 ~ 1.5; Vitrified bond consists of 23 μ m silicon carbide, chromatographic aluminium oxide, magnesium oxide, and mass ratio is 10:0.5 ~ 6.5:0 ~ 2; Take by weighing 0.5 ~ 15g Xylo-Mucine again, the water-bath magnetic agitation is even in the deionized water of adding 40 ~ 300ml, add aluminum silicate fiber, mullite fiber, vitrified bond successively, stir in the time of heated and boiled, until fiber dispersion evenly and make that the mullite fiber massfraction is 1 ~ 10% in the slurry, can obtain fiber and binding agent mixed slurry;
(3) uniform fiber layer slurry obtains: with step (2) prepare fiber and binding agent compound adding 10 ~ 100g ball-milling medium, put into ball mill with 50 ~ 400 rev/mins of rotating speed ball millings 10 ~ 400 minutes, can obtain uniformly dispersing fibre layer slurry;
(4) step (3) is prepared uniformly dispersing fibre layer slurry pour in the paint sprayer, adjust intake pressure, nozzle subtended angle, walk rifle speed, slurry speed, flour milling thickness, planeness are inhaled in control, make layer of fibers evenly be coated on the supporter, rotary supporting body, spraying reaches required fiber layer thickness continuously; It is standby to put into 110 ℃ of oven dry of baking oven, 6 ~ 24h after the spraying;
(5) coating liquid preparing solvent: be 0 ~ 30:0 ~ 40:0 ~ 90:0 ~ 80:0 ~ 25 weighings by glycerol, propylene glycol, ethanol, ethylene glycol, triethylene glycol volume ratio, pour in the beaker, utilize magnetic stirring apparatus to mix and stir 5 ~ 100min;
(6) preparation of vitrified bond: be that 65wt% potassium felspar sand, 12wt% burn kaolin and the preparation of 23wt% white carbon black by massfraction, utilize ethanol as solvent, agate ball is as ball-milling medium, and wherein material and ball-milling medium and ethanol mass ratio are 1:3:4.5; After utilizing planetary ball mill with 300 rev/mins of ball milling 70h of rotating speed, at 110 ℃ of following oven dry 12h, obtain the film adhesive that glassy phase is main body behind 300 mesh sieves excessively; Or be that 0.5-30 μ m aluminum oxide powder is film adhesive with the particle diameter; Or be film adhesive with the aluminium hydrate powder; Or to mix ceramics powder by 3 ~ 6:0.1 ~ 3 mass ratioes through ball milling with aluminum oxide and magnesium oxide be film adhesive;
(7) even filtering membrane pulp preparation: the mass ratio by carborundum powder, vitrified bond, pore-forming material and coating liquid solvent is 10:0.5 ~ 3.3:0 ~ 4.0:10 ~ 100, take by weighing the required amount of each raw material respectively, add carborundum powder, vitrified bond, pore-forming material stirring 20 ~ 70min again in the uniform coating liquid solvent in step (5) successively, thereby obtain uniform filtering membrane slurry; In the described preparation filtering membrane slurry, the grain diameter of carborundum powder is 1 ~ 30 μ m, and the vitrified bond grain diameter is 0.1 ~ 60 μ m, and content is 5 ~ 25wt%;
(8) the filtering membrane slurry applies: even filtering membrane slurry is poured in the paint sprayer, adjust intake pressure, nozzle subtended angle, walk rifle speed, make filtering membrane evenly be coated on the supporter, in the spraying process supporter is put on the turntable of constant speed rotation, spraying continuously reaches required filtering membrane thickness by the control spray time; Be put into 110 ℃ of oven dry of baking oven, 6 ~ 48h after the spraying, oven dry 6 ~ 48h is standby down at 160-240 ℃ again;
(9) sintering of composite filter material: with even coated filtering material sintering, sintering temperature is 1250 ~ 1550
oC, temperature rise rate 2 ~ 20
oC/min, soaking time is 1 ~ 6h.
Composite silicon carbide ceramic filter membrane material of the present invention is to spray one deck silicon carbide film material on the silicon carbide ceramics supporter of fiber transition layer again scribbling.Stable dispersion, viscosity are suitable by making, the coating liquid of good film-forming property, and it is evenly complete to utilize the aerial spraying technology to obtain, the large size silicon-carbide mineral membrane of controllable thickness.This method not only technology simple operations is convenient, can film to the large size filtering material simultaneously, is easy to realize suitability for industrialized production.
Description of drawings
The SEM figure of Fig. 1 binding agent filtering membrane sintering rear surface based on glassy phase provided by the invention;
Fig. 2 is provided by the invention to be the SEM figure of binding agent filtering membrane sintering rear surface with the chromatographic aluminium oxide;
Fig. 3 is provided by the invention with aluminium hydroxide be binding agent filtering membrane sintering rear surface SEM figure;
The SEM of three-decker section figure behind Fig. 4 composite silicon carbide ceramic material provided by the invention sintering;
The SEM figure of Fig. 5 composite silicon carbide ceramic material provided by the invention sintering after-filtration film section;
Embodiment
Embodiment 1
(1) mass ratio by carborundum powder, vitrified bond, pore-forming material and Xylo-Mucine (CMC) solution is 10:1.1:0.4:1.4, take by weighing the required amount of each raw material respectively, with dry-pressing formed after its mixing and stirring, pressure is that 5MPa prepares supporter green compact diameter 50mm, and thickness is about 5mm.Wherein the median size of silicon-carbide particle is 150 μ m, and the mass concentration of Xylo-Mucine (CMC) solution is 1.5wt%, and pore-forming material is graphite, and binding agent is for pressing 65wt% potassium felspar sand, 12wt% kaolin and 23wt% quartz sand ball milling compound.
(2) supporter sintering is with the green compact dry 24h in 110 ℃ of baking ovens for preparing, with temperature rise rate 20
oC/min sinters to 1200 ℃, and soaking time is 1h.
(3) take by weighing length respectively at the mullite fiber 2g of 1 ~ 2cm, aluminum silicate fiber 1.8g, sodium cellulose glycolate 2g, binding agent 1g, the deionized water that takes by weighing 70ml adds in the 250ml beaker, stirring in water bath, add Xylo-Mucine, aluminum silicate fiber successively, mullite fiber, binding agent, heating in water bath stirs, and causes the mullite fiber mass concentration and reaches 4%.The layer of fibers binding agent is that 23 μ m silicon carbide and chromatographic aluminium oxide and magnesium oxide mix by mass ratio 9:4:0.3.
(4) add the 30g ball-milling medium at fiber and binding agent compound, put into planetary ball mill with 250 rev/mins rotating speed ball milling 20 minutes, ball-milling medium is the agate ball about diameter 0.5cm, can obtain the uniformly dispersing fibre slurry.
(6) the uniform fiber slurry is poured in the watering can, utilized aerial spraying, evenly be sprayed on supporting body surface, be placed into 110 ℃ of dry 10h in the baking oven.
(7) the coating liquid solvent is the 20:20:20:20:20 preparation by triethylene glycol, ethanol, ethylene glycol, glycerol, propylene glycol volume ratio.Weighing quality respectively is that 65g potassium felspar sand, 12g burn kaolin and 23g white carbon black, utilizes ethanol as solvent, and agate ball is as ball-milling medium, and wherein material and ball-milling medium and ethanol mass ratio are 1:3:4.5.After utilizing planetary ball mill with 300 rev/mins of ball milling 70h of rotating speed, mistake 300 mesh sieves obtain the film adhesive based on glassy phase behind 100 ℃ of following oven dry 10h.
The even dispersing and filtering film slurry that (8) will prepare is poured in the paint sprayer, adjust intake pressure, nozzle subtended angle, walk rifle speed etc., thereby slurry speed, flour milling thickness, planeness is inhaled in control, filtering membrane evenly is coated in scribbles on the fibrolaminar supporter.Rotary supporting body, spraying reaches required filtering membrane thickness continuously;
(9) with the filtering material dry 20h in 110 ℃ of baking ovens for preparing, dry 8h down at 200 ℃ again, then composite silicon carbide ceramic filter membrane material base substrate to be calcined, sintering temperature is 1400
oC, temperature rise rate 5
oC/min, insulation 2h can make the composite silicon carbide ceramic filter membrane material.
(10) result: its surperficial SEM Photomicrograph of composite silicon carbide ceramic as shown in Figure 1; Can obtain surperficial complete, the relatively more uniform filtering membrane of pore size distribution, the mean porosities 45.3% of filtering membrane, mean pore size 1.9 μ m;
Embodiment 2
(1) with step (1) ~ (6) of embodiment 1
(2) the coating liquid solvent is 15:35:50 by propylene glycol, ethanol, ethylene glycol volume ratio;
(3) with 300 order chromatographic aluminium oxides as binding agent;
(4) mass ratio by carborundum powder, vitrified bond, coating liquid is 10:3:40, take by weighing the required amount of each raw material respectively, at first coating liquid is added in the beaker, add carborundum powder successively again, vitrified bond utilizes magnetic agitation, thereby obtain uniform filtering membrane slurry; In the described preparation filtering membrane slurry, the grain diameter of carborundum powder is 23.1 μ m, and chromatographic aluminium oxide adhesive particle particle diameter is 0.1 ~ 19 μ m;
(5) with the step (8) of embodiment 1
(6) will prepare filtering material dry 12h in 110 ℃ of baking ovens, dry 10h down at 200 ℃ again, the composite silicon carbide ceramic filter membrane material be calcined sintering temperature 1350
oC, temperature rise rate 5
oC/min, soaking time 3h can make the composite silicon carbide ceramic filter membrane material.
(7) result: its surperficial SEM Photomicrograph of composite silicon carbide ceramic as shown in Figure 2: filter membrane surface is smooth, the even aperture distribution defective is few.
Embodiment 3
(1) with step (1) ~ (6) of embodiment 1;
(2) the coating liquid solvent is 10:10:20:60 by triethylene glycol, glycerol, ethanol, ethylene glycol volume ratio;
(3) with aluminium hydroxide as binding agent;
(4) mass ratio by carborundum powder, vitrified bond, coating liquid is 10:3:50, take by weighing the required amount of each raw material respectively, at first coating liquid is added in the beaker, add carborundum powder successively again, vitrified bond utilizes magnetic agitation, thereby obtain uniform filtering membrane slurry; In the described preparation filtering membrane slurry, the grain diameter of carborundum powder is 7.6 μ m, and aluminium hydroxide adhesive particle particle diameter is 0.1 ~ 11 μ m;
(5) with the step (8) of embodiment 1
(6) will prepare filtering material dry 12h in 110 ℃ of baking ovens, dry 12h down at 200 ℃ again, the composite silicon carbide ceramic filter membrane material be calcined sintering temperature 1350
oC, temperature rise rate 5
oC/min, soaking time 2h can make the composite silicon carbide ceramic filter membrane material.
(7) result: filter membrane surface SEM Photomicrograph as shown in Figure 3: filter membrane surface is smooth, the even aperture distribution defective is few.Complex silicon carbide filtering material section SEM Photomicrograph is as shown in Figure 4: the ceramic fiber transition layer has played to build bridge accepts effect, prevent that effectively film from directly contacting supporter and stopping up pore, supporter, ceramic fiber transition layer and surface carborundum film are connected closely upper layer filtering membrane difficult drop-off owing to add the vitrified bond three in layer of fibers; Filtering membrane section SEM Photomicrograph is as shown in Figure 5: have high pore connectivity when filtering membrane has good combination.
Above disclosed only is preferred embodiment of the present invention, can not limit the present invention's interest field certainly with this, and therefore the equivalent variations of doing according to claim of the present invention still belongs to the scope that the present invention is contained.
Claims (1)
1. high temperature filtration is with the coating method of silicon carbide ceramics film, comprise preparation carborundum porous ceramics supporter base substrate, preparation layer of fibers slurry, preparation uniform fiber layer slurry, the coating of uniform fiber layer slurry, filtering membrane pulp preparation and filtering membrane slurry coating step, it is characterized in that: filtering membrane pulp preparation and filtering membrane slurry apply and are specially following steps:
(1) coating liquid preparing solvent: be 0 ~ 30:0 ~ 40:0 ~ 90:0 ~ 80:0 ~ 25 weighings by glycerol, propylene glycol, ethanol, ethylene glycol, triethylene glycol volume ratio, pour in the beaker, utilize magnetic stirring apparatus to mix and stir 5 ~ 100min;
(2) preparation of vitrified bond: be that 65wt% potassium felspar sand, 12wt% burn kaolin and the preparation of 23wt% white carbon black by massfraction, utilize ethanol as solvent, agate ball is as ball-milling medium, and wherein material and ball-milling medium and ethanol mass ratio are 1:3:4.5; After utilizing planetary ball mill with 300 rev/mins of ball milling 70h of rotating speed, at 110 ℃ of following oven dry 12-30h, obtain the film adhesive that glassy phase is main body behind 300 mesh sieves excessively; Or be that 0.5-30 μ m aluminum oxide powder is film adhesive with the particle diameter; Or be film adhesive with the aluminium hydrate powder; Or to mix ceramics powder by 3 ~ 6:0.1 ~ 3 mass ratioes through ball milling with aluminum oxide and magnesium oxide be film adhesive;
(3) even filtering membrane pulp preparation: the mass ratio by carborundum powder, vitrified bond, pore-forming material and coating liquid solvent is 10:0.5 ~ 3.3:0 ~ 4.0:10 ~ 100, take by weighing the required amount of each raw material respectively, add carborundum powder, vitrified bond, pore-forming material stirring 20 ~ 70min successively in the uniform coating liquid solvent in step (1) successively again, thereby obtain uniform filtering membrane slurry; In the described preparation filtering membrane slurry, the grain diameter of carborundum powder is 1 ~ 30 μ m, and the vitrified bond grain diameter is 0.1 ~ 60 μ m, and content is 5 ~ 25wt%;
(4) the filtering membrane slurry applies: even filtering membrane slurry is poured in the paint sprayer, adjust intake pressure, nozzle subtended angle, walk rifle speed, make filtering membrane evenly be coated on the supporter, in the spraying process supporter is put on the turntable of constant speed rotation, spraying continuously reaches required filtering membrane thickness by the control spray time; Put into 110 ℃ of oven dry of baking oven, 6 ~ 48h after the spraying, oven dry 6 ~ 48h is standby down at 160-240 ℃ again;
(5) sintering of composite filter material: with even coated filtering material sintering, sintering temperature is 1250 ~ 1550
oC, temperature rise rate 2 ~ 20
oC/min, soaking time is 1 ~ 6h.
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Cited By (9)
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| CN103482999A (en) * | 2013-09-29 | 2014-01-01 | 陈春水 | High-permeability porous ceramic membrane and preparation method thereof |
| CN104475307A (en) * | 2014-11-10 | 2015-04-01 | 华玉叶 | Mechanical membrane spraying technique |
| CN105921030A (en) * | 2016-06-28 | 2016-09-07 | 董超超 | Gas filter composite membrane |
| CN106178976A (en) * | 2016-06-28 | 2016-12-07 | 董超超 | A kind of filter membrane containing titanium dioxide granule |
| CN106390772A (en) * | 2016-09-20 | 2017-02-15 | 芜湖成德龙过滤设备有限公司 | Ceramic filter membrane and preparation method thereof |
| CN108329033A (en) * | 2018-01-26 | 2018-07-27 | 山东理工大学 | Liquid-phase sintering multichannel silicon carbide ceramics membrane component and preparation method thereof |
| CN108395252A (en) * | 2018-01-26 | 2018-08-14 | 山东理工大学 | Liquid-phase sintering multichannel silicon carbide ceramic support body and preparation method thereof |
| CN109847468A (en) * | 2019-01-16 | 2019-06-07 | 苏州宏久航空防热材料科技有限公司 | A kind of two dimension silicon carbide fiber cloth reinforced composite material screen pipe |
| CN115430297A (en) * | 2022-11-08 | 2022-12-06 | 山东赛利科膜科技有限公司 | Silicon carbide ceramic membrane for heavy metal wastewater treatment and production method thereof |
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| CN106178976A (en) * | 2016-06-28 | 2016-12-07 | 董超超 | A kind of filter membrane containing titanium dioxide granule |
| CN106390772A (en) * | 2016-09-20 | 2017-02-15 | 芜湖成德龙过滤设备有限公司 | Ceramic filter membrane and preparation method thereof |
| CN108329033A (en) * | 2018-01-26 | 2018-07-27 | 山东理工大学 | Liquid-phase sintering multichannel silicon carbide ceramics membrane component and preparation method thereof |
| CN108395252A (en) * | 2018-01-26 | 2018-08-14 | 山东理工大学 | Liquid-phase sintering multichannel silicon carbide ceramic support body and preparation method thereof |
| CN109847468A (en) * | 2019-01-16 | 2019-06-07 | 苏州宏久航空防热材料科技有限公司 | A kind of two dimension silicon carbide fiber cloth reinforced composite material screen pipe |
| CN109847468B (en) * | 2019-01-16 | 2021-04-02 | 苏州宏久航空防热材料科技有限公司 | Two-dimensional silicon carbide fiber cloth reinforced ceramic matrix composite filter pipe |
| CN115430297A (en) * | 2022-11-08 | 2022-12-06 | 山东赛利科膜科技有限公司 | Silicon carbide ceramic membrane for heavy metal wastewater treatment and production method thereof |
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