CN107511077A - A kind of preparation method of industrial air filter filter membrane - Google Patents

A kind of preparation method of industrial air filter filter membrane Download PDF

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Publication number
CN107511077A
CN107511077A CN201710992280.2A CN201710992280A CN107511077A CN 107511077 A CN107511077 A CN 107511077A CN 201710992280 A CN201710992280 A CN 201710992280A CN 107511077 A CN107511077 A CN 107511077A
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preparation
filter membrane
powder
parts
compound
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冷祥珠
龚圣杰
王伟
江训林
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JIANGSU HUAQIANG NEW ENERGY TECHNOLOGY Co Ltd
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JIANGSU HUAQIANG NEW ENERGY TECHNOLOGY Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0079Manufacture of membranes comprising organic and inorganic components
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D46/00Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/54Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
    • B01D46/543Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/22Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
    • B01D53/228Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0081After-treatment of organic or inorganic membranes
    • B01D67/0095Drying
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12Composite membranes; Ultra-thin membranes

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Filtering Materials (AREA)

Abstract

The invention discloses a kind of preparation method of industrial air filter filter membrane, the preparation method of the filter membrane comprises the following steps:(1)The preparation of vitrified bonding-(2)The preparation of carboxymethylcellulose sodium solution-(3)The preparation of compound support-(4)The preparation of ceramic fibre transition zone-(5)The preparation of filter membrane;The preparation method is simple and easy, and preparation technology has very high antifalsification, the filter membrane even structure prepared, has good high temperature resistant, high pressure and chemical stability, filtration pressure is reduced, increased the service life.

Description

A kind of preparation method of industrial air filter filter membrane
Technical field
The invention belongs to daily-use chemical industry filtration art, and in particular to a kind of system of industrial air filter filter membrane Preparation Method.
Background technology
Air is the existing guarantee that sustains life, and contains substantial amounts of pernicious gas and tiny suspended particulate substance in air, The respiratory tract, angiocarpy and central nervous system of human breathing immunologic function can all be caused to seriously endanger, cut down in air and hang The discharge capacity of floating particles thing to environmental protection, ensure health be it is vital, at present, with industry fast development, Environment for human survival is constantly challenged, and one of them is exactly air pollution;Meanwhile modern science and modern industry, particularly The development of the industry such as the industry such as electronics, precision instrument, metallurgy, aerospace, nuclear energy, chemical industry and medical treatment, pharmacy, food, to technique The air purity of environment it is also proposed higher requirement, and high-temperature flue gas purification has turned into the row such as material, metallurgy, chemical industry, electric power Industry realizes an important technology brainstorm subject of " energy-saving and emission-reduction ", and many industrial smokes belong to high-temperature flue gas, such as smelt, burn, Thermal power generation etc., at present, it is exactly to air filtration to solve this air quality problems most efficient method, and filter membrane is air Critical elements in filter, it is referred to as the heart of filter, whether up to standard is directly connected to particulate in air concentration Key factor.
Although traditional filter membrane has higher filter efficiency to particle more than micron order, it is difficult to Asia Effective filtering of micron particles, at the same the fiber filter film sold on the market typically can not all reach simultaneously Chalk-dust filtering and Oiliness particle, essentially consisting in filter membrane typically can not all reach hydrophobic, oleophobic effect simultaneously, and research shows fiber filter film Filter efficiency can significantly improve with the reduction of fibre diameter, thus, reducing fibre diameter turns into improvement fiber filter film A kind of effective ways, electrostatic spinning technique can prepare diameter superfine fibre in several nanometers to several micrometer ranges as a kind of Method, attracted wide attention in the preparation of fiber filter film, in addition to fibre diameter is small, by electrostatic spinning technique system The fibrous material obtained also has the advantages that aperture is small, voidage is high, fiber homogeneity is good, it is filtered in gas filtration, liquid And the field such as individual protection shows huge potential application;Therefore, develop a kind of industrial air filter is with filter membrane The problem of those skilled in the art's urgent need to resolve.
The content of the invention
The technical problems to be solved by the invention are the shortcomings that presence for above prior art, propose that a kind of industry is empty The preparation method of air filter filter membrane, the preparation method is simple and easy, and preparation technology has very high antifalsification, prepares Filter membrane even structure, there is good high temperature resistant, high pressure and chemical stability, filtration pressure is reduced, extend use Life-span.
The present invention solve above technical problem technical scheme be:
A kind of preparation method of industrial air filter filter membrane, the preparation method of the filter membrane comprise the following steps:
(1)The preparation of vitrified bonding
By water based acrylic resin, kaolin, silica sand, silica, dispersant, calcium carbonate, coupling agent, thickener and answer Rare earth is closed, is well mixed, then carries out ball milling, ball milling 30-35h, ball milling speed 400-450t/min, is put into drying after ball milling Dry, pulverize at 50-60 DEG C in case, you can obtain vitrified bonding powder;
(2)The preparation of carboxymethylcellulose sodium solution
Sodium carboxymethylcellulose powder is put into container, deionized water is added, boils under magnetic stirring, until obtaining dense Spend the carboxymethylcellulose sodium solution for 2wt%;
(3)The preparation of compound support
Carborundum is calcined at 800-1000 DEG C, 2-3h is then soaked in hydrogen peroxide solution, after taking-up is rinsed well 300 microns of silicon-carbide particle is chosen in screening;
By 300 microns of silicon-carbide particle and step(2)The carboxymethylcellulose sodium solution prepared is sufficiently mixed, in mass ratio Count carboxymethylcellulose sodium solution:Silicon-carbide particle=1:7-9, until carboxymethylcellulose sodium solution is on silicon-carbide particle surface Form one layer of uniform solution layer;
Using a small amount of multiple method by step(1)The vitrified bonding powder of middle preparation adds surface and forms carboxymethyl cellulose In the sic powder of sodium solution layer, it is stirred continuously until vitrified bonding powder is evenly coated at silicon-carbide particle surface;
Pore creating material powder is continuously added, and is stirred, pore creating material powder is distributed in the pottery for being coated on silicon-carbide particle surface Between the outside of porcelain binding agent and particle;
The powder of preparation is subjected to dry-pressing formed, pressure 20-24MPa, be supported body base substrate, and base substrate is sintered, and is burnt Junction temperature is 1200-1300 degrees Celsius, is incubated 1-2h, mean porosities 35-38%, a diameter of 40-50mm, after natural cooling Supporter side can obtain compound support in 100-120 DEG C of compound nonwoven cloth substrate layer;
(4)The preparation of ceramic fibre transition zone
Aluminium silicate fiber peacekeeping mullite fiber is mixed and uses magnetic agitation is scattered to mix, then adds sodium cellulose glycolate And deionized water, continue to be well mixed, then carry out ball milling and can obtain uniform ceramic fibre transition zone slurry;
Alumina silicate fibre is counted in mass ratio:Mullite fiber:Sodium carboxymethylcellulose:Deionized water=1:1.5:1.5:65(There is original Cause)
By ceramic fibre transition zone slurry using tape casting machine on the compound support prepared away from non-woven fabrics base material layer Side casting film-forming, obtained base film is dried in an oven, it is about 100-110 microns that repeatedly 3-4 times, which obtains thickness, according to this Ceramic interlayer film;
(5)The preparation of filter membrane
By the sic powder, vitrified bonding, deionized water of 20-25 microns, sodium carboxymethylcellulose is well mixed, obtained Filter membrane compound;
Sic powder is counted in mass ratio:Vitrified bonding:Deionized water:Sodium carboxymethylcellulose=10:1:4:2;
In step(4)Casting film-forming is carried out using filter membrane compound on the ceramic interlayer film surface prepared, by what is obtained 3-5 curtain coating obtains the silicon carbide ceramics filter membrane that thickness is 300-350 microns to the drying of transition tunic repeatedly, in 1300-1400 It is sintered under degree Celsius and can obtain filter membrane after being incubated 2-3h.
The technical scheme that further limits of the present invention as:
In the preparation method of aforementioned industrial air cleaner filter membrane, filter membrane is compound with graphene, and concrete operations are:
Configuration concentration is 0.005-8mg/ml graphene oxide solution, using press filtration mode by graphene oxide solution along vertically In step(5)The direction of the filter membrane prepared is permeated in the micropore of the surface of filter membrane and filter membrane;
And reaction 5-10h is carried out under an inert atmosphere using sodium borohydride or hydroiodic acid, obtains combined filtration at 700-1200 DEG C Film.
In the preparation method of aforementioned industrial air cleaner filter membrane, step(1)Middle vitrified bonding presses mass fraction Meter includes following components:
Water based acrylic resin:30-40 parts, kaolin:20-25 parts, silica sand:10-15 parts, silica:10-13 parts, Dispersant:5-7 parts, calcium carbonate:1-3 parts, coupling agent:4-6 parts, thickener:3-5 parts, compound rare-earth:0.1-0.3 parts;
Compound rare-earth includes following component by weight percentage:Y:13%, Sc:16%, Gd:9%, Sm:18%, Pr:9%, surplus is La, above each component sum are 100%;
Coupling agent is at least one of silane coupler or zirconium class coupling agent;Dispersant is calgon;Thickener is swollen Profit soil, attapulgite or alumina silicate.
Technique effect, has used kaolin in binding agent, and kaolin has a whiteness and brightness, granularity point, plasticity, with reference to Property, viscosity and thixotropy, drying property, agglutinating property burn till contractions, fire resistance, suspension and dispersiveness, washability, ion suction Attached property and exchangeability, chemical stability and electrical insulating property;
Silica sand is a kind of hard, wear-resisting, stable chemical performance cinnamic acid salt mineral, and its chemistry, calorifics and mechanical performance have bright Aobvious anisotropy, insoluble in acid, it is slightly soluble in KOH solution;
The present invention with the addition of dispersant, and dispersant can increase the compatibility between base-material, can prevent that particle wadding is poly-, reduce binding agent and stick Degree, is firmly adsorbed on the surface of dispersed particle, and provides good space repulsion, particle is fully divided under high velocity agitation Dissipate after, will not reunite again because of Van der Waals force, adsorption layer also will not when being acted on by external force from particle surface peel off and Cause the unstable of system, so as to optimize the physics of binding agent and chemical property;
Add compound rare-earth in binding agent of the present invention, due to the metallic atomic radius of above rare earth element is big and rare earth have compared with High activity, it is easy to fill up the space of storeroom, meanwhile, rare earth element easily and the element compounds such as oxygen, sulphur to generate fusing point high Compound, the addition of compound rare-earth improve the dispersiveness and compatibility that prepare binding agent, make product mix to a certain extent Uniformly also improve the anti-flammability of binding agent.
In the preparation method of aforementioned industrial air cleaner filter membrane, the preparation method of water based acrylic resin For:
N-butanol is added into the three-necked flask equipped with agitator agent water-bath, is heated up to 90-95 DEG C, then by benzoyl peroxide first Acyl is dissolved in methyl methacrylate, hydroxy-ethyl acrylate, the mixed liquor of acryloid lauryl mercaptan, and by mixed liquor be added dropwise into In three-necked flask, dropwise addition maintains 3-4h completions, and controls temperature after being added dropwise and being incubated 1-2h, to be added at 90-95 DEG C BP is simultaneously warming up to 100-110 DEG C, insulation 0.5-1h, and then triethylamine, regulation is added dropwise to 35-45 DEG C in slow cooling PH value heats removed under reduced pressure partial solvent, finally, adds water dilution and obtain water based acrylic resin to 7.5-8.
In the preparation method of aforementioned industrial air cleaner filter membrane, step(3)By 300 microns after screening of carborundum Powder is pre-processed, by sic powder, aluminum oxide abrading-ball and water in mass ratio 1:1:1.5 ratio is added in ball grinder, Then ball milling 20-24h under 140-150 revs/min of rotating speed again, the sic powder after ball milling is dried, screening obtains 300 microns Carborundum.
In the preparation method of aforementioned industrial air cleaner filter membrane, the thickness of non-woven fabrics base material layer is 500-700 μm.
In the preparation method of aforementioned industrial air cleaner filter membrane, step(3)Middle pore creating material be flake graphite in powder and The mixture of activated carbon, counts flake graphite in powder in mass ratio:Activated carbon=1:1.5.
In the preparation method of aforementioned industrial air cleaner filter membrane, step(4)In aluminium silicate fiber peacekeeping mullite The length of fiber is trimmed to 10mm and 20mm respectively.
The beneficial effects of the invention are as follows:
Carborundum is employed herein, carborundum has very high molten point, bending strength, fracture toughness and thermal conductivity, together When there is relatively low thermal coefficient of expansion and density, be that a kind of elevated temperature strength is good, thermal shock resistance is strong, thermal conductivity is good and the pottery of corrosion resistant candle Ceramic material;
Active powdered carbon, because microcrystalline carbon is irregular alignment, there is pore in structure between interconnection, can be produced in activation Raw carbon tissue defects, therefore it is a kind of porous carbon, bulk density is low, and specific surface area is big, and this assay activity charcoal is pore creating material.
Sodium carboxymethylcellulose has excellent dispersion force and adhesion, and its aqueous solution can make emulsifying agent with alkaline solution, Also there is emulsifying capacity to oil and wax, be a kind of powerful emulsifying agent, the aqueous solution of sodium carboxymethylcellulose to thermally labile, its Viscosity reduces with the rise of temperature.
The polycrystalline mullite fibre used in transition zone can be used in less than 1600 °C of high temperature Thermal Equipment make for a long time Heat-insulating material, equipment thermal efficiency is remarkably improved, significantly saves the energy, improved productivity ratio, improve production quality.
Sintering temperature is reduced present invention adds vitrified bonding and prepares porous ceramics, is reduced energy consumption, is easy to be commercialized A large amount of productions.
The present invention is provided with ceramic fibre transition zone, the filtering containing ceramic fibre transition zone between matrix and filter layer Film surface is relatively smooth, and the filter membrane surface without ceramic fibre filtering is rough, because porous ceramic support Surface holes it is more and rough smooth, be unfavorable for film, coat transition thickness, the transition provides more smooth as film Surface, and the presence of transition zone can ensure that filter membrane slurry will not enter supporter space, without the filter membrane of transition zone Slurry can be blocked largely in supporter space, influence the filter efficiency of filter membrane.
Using carborundum as primary raw material, add vitrified bonding and sic powder is bonded to membrane filtration after high temperature sintering Film advantageously reduces the thermal stress of the two interface with supporter using same material system, reduces the heat fatigue of filtering film layer Damage.
The present invention also designs a kind of composite filtering film, and graphene oxide is compound with ceramics, and the method can will aoxidize stone Black alkene solution is penetrated into the micropore of ceramic filtration membrane, avoids adsorbing the aperture size on surface, reducing micropore in ceramic membrane, and Graphene oxide is carried out to be reduced into graphene so as to be chemically bound together between graphene and ceramic filtration membrane, by stone The filterability of black alkene is attached in ceramic filtration membrane, is added filter efficiency, composite membrane high mechanical strength, good filtration effect, is benefited from Long lifespan.
Embodiment
Embodiment 1
The present embodiment provides a kind of preparation method of industrial air filter filter membrane, the preparation method of the filter membrane include with Lower step:
(1)The preparation of vitrified bonding
By water based acrylic resin, kaolin, silica sand, silica, dispersant, calcium carbonate, coupling agent, thickener and answer Rare earth is closed, is well mixed, then carries out ball milling, ball milling 30h, ball milling speed 400t/min, is put into drying baker after ball milling Dry, pulverize at 50 DEG C, you can obtain vitrified bonding powder;
Step(1)Middle vitrified bonding includes following components according to the mass fraction:
Water based acrylic resin:30 parts, kaolin:20 parts, silica sand:10 parts, silica:10 parts, dispersant:5 parts, carbon Sour calcium:1 part, coupling agent:4 parts, thickener:3 parts, compound rare-earth:0.1 part;
Compound rare-earth includes following component by weight percentage:Y:13%, Sc:16%, Gd:9%, Sm:18%, Pr:9%, surplus is La, above each component sum are 100%;
Coupling agent is silane coupler;Dispersant is calgon;Thickener is bentonite;
The preparation method of water based acrylic resin is:
N-butanol is added into the three-necked flask equipped with agitator agent water-bath, is heated up to 90 DEG C, then by benzoyl peroxide Methyl methacrylate, hydroxy-ethyl acrylate, the mixed liquor of acryloid lauryl mercaptan are dissolved in, and mixed liquor is added dropwise into three In mouth flask, dropwise addition maintains 3h completions, and controls temperature after being added dropwise and being incubated 1h, to add benzoyl peroxide first at 90 DEG C Acyl is simultaneously warming up to 100 DEG C, insulation 0.5h, and then triethylamine, regulation pH value to 7.5, heating decompression is added dropwise to 35 DEG C in slow cooling Partial solvent is removed, finally, water dilution is added and obtains water based acrylic resin;
(2)The preparation of carboxymethylcellulose sodium solution
Sodium carboxymethylcellulose powder is put into container, deionized water is added, boils under magnetic stirring, until obtaining dense Spend the carboxymethylcellulose sodium solution for 2wt%;
(3)The preparation of compound support
Carborundum is calcined at 800 DEG C, 2h is then soaked in hydrogen peroxide solution, taking-up is sieved after rinsing well and chosen 300 microns of silicon-carbide particle;
Sic powder is pre-processed, by sic powder, aluminum oxide abrading-ball and water in mass ratio 1:1:1.5 ratio adds Enter in ball grinder, then ball milling 20h under 140 revs/min of rotating speed again, the sic powder after ball milling is dried;
By 300 microns of silicon-carbide particle and step(2)The carboxymethylcellulose sodium solution prepared is sufficiently mixed, in mass ratio Count carboxymethylcellulose sodium solution:Silicon-carbide particle=1:7, until carboxymethylcellulose sodium solution is in silicon-carbide particle surface shape Into one layer of uniform solution layer;
Using a small amount of multiple method by step(1)The vitrified bonding powder of middle preparation adds surface and forms carboxymethyl cellulose In the sic powder of sodium solution layer, it is stirred continuously until vitrified bonding powder is evenly coated at silicon-carbide particle surface;
Pore creating material powder is continuously added, and is stirred, pore creating material powder is distributed in the pottery for being coated on silicon-carbide particle surface Between the outside of porcelain binding agent and particle;
Pore creating material is the mixture of flake graphite in powder and activated carbon, counts flake graphite in powder in mass ratio:Activated carbon=1:1.5;
The powder of preparation is subjected to dry-pressing formed, pressure 20MPa, be supported body base substrate, and base substrate is sintered, sintering temperature Spend for 1200 degrees Celsius, be incubated 1h, mean porosities 35%, a diameter of 40mm, natural cooling rear supports side is at 100 DEG C The non-woven fabrics base material layer that composite thickness is 500 μm can obtain compound support;
(4)The preparation of ceramic fibre transition zone
The length of first aluminium silicate fiber peacekeeping mullite fiber is trimmed to 10mm and 20mm respectively, and aluminium silicate fiber peacekeeping mullite is fine Dimension is mixed and mixed using magnetic agitation is scattered, is then added sodium cellulose glycolate and deionized water, is continued to be well mixed, so Ball milling is carried out afterwards can obtain uniform ceramic fibre transition zone slurry;
Alumina silicate fibre is counted in mass ratio:Mullite fiber:Sodium carboxymethylcellulose:Deionized water=1:1.5:1.5:65;
By ceramic fibre transition zone slurry using tape casting machine on the compound support prepared away from non-woven fabrics base material layer Side casting film-forming, obtained base film is dried in an oven, is repeated 3 times to obtain the ceramics that thickness is about 100 microns according to this Transition tunic;
(5)The preparation of filter membrane
By 20 microns of sic powder, vitrified bonding, deionized water, sodium carboxymethylcellulose is well mixed, filtered Film compound;
Sic powder is counted in mass ratio:Vitrified bonding:Deionized water:Sodium carboxymethylcellulose=10:1:4:2;
In step(4)Casting film-forming is carried out using filter membrane compound on the ceramic interlayer film surface prepared, by what is obtained 3 curtain coatings obtain the silicon carbide ceramics filter membrane that thickness is 300 microns to the drying of transition tunic repeatedly, are carried out under 1300 degrees Celsius Sinter and can obtain filter membrane after being incubated 2h.
Embodiment 2
The present embodiment provides a kind of preparation method of industrial air filter filter membrane, the preparation method of the filter membrane include with Lower step:
(1)The preparation of vitrified bonding
By water based acrylic resin, kaolin, silica sand, silica, dispersant, calcium carbonate, coupling agent, thickener and answer Rare earth is closed, is well mixed, then carries out ball milling, ball milling 35h, ball milling speed 450t/min, is put into drying baker after ball milling Dry, pulverize at 50-60 DEG C, you can obtain vitrified bonding powder;
Step(1)Middle vitrified bonding includes following components according to the mass fraction:
Water based acrylic resin:40 parts, kaolin:25 parts, silica sand:15 parts, silica:13 parts, dispersant:7 parts, carbon Sour calcium:3 parts, coupling agent:6 parts, thickener:5 parts, compound rare-earth:0.3 part;
Compound rare-earth includes following component by weight percentage:Y:13%, Sc:16%, Gd:9%, Sm:18%, Pr:9%, surplus is La, above each component sum are 100%;
Coupling agent is zirconium class coupling agent;Dispersant is calgon;Thickener is attapulgite;
The preparation method of water based acrylic resin is:
N-butanol is added into the three-necked flask equipped with agitator agent water-bath, is heated up to 95 DEG C, then by benzoyl peroxide Methyl methacrylate, hydroxy-ethyl acrylate, the mixed liquor of acryloid lauryl mercaptan are dissolved in, and mixed liquor is added dropwise into three In mouth flask, dropwise addition maintains 4h completions, and controls temperature after being added dropwise and being incubated 2h, to add benzoyl peroxide first at 95 DEG C Acyl is simultaneously warming up to 110 DEG C, insulation 1h, and then slow cooling is added dropwise triethylamine, regulation pH value to 8, heats removed under reduced pressure to 45 DEG C Partial solvent, finally, add water dilution and obtain water based acrylic resin;
(2)The preparation of carboxymethylcellulose sodium solution
Sodium carboxymethylcellulose powder is put into container, deionized water is added, boils under magnetic stirring, until obtaining dense Spend the carboxymethylcellulose sodium solution for 2wt%;
(3)The preparation of compound support
Carborundum is calcined at 1000 DEG C, 3h is then soaked in hydrogen peroxide solution, rear screening and choosing is rinsed in taking-up well Take 300 microns of silicon-carbide particle;
Sic powder is pre-processed, by sic powder, aluminum oxide abrading-ball and water in mass ratio 1:1:1.5 ratio adds Enter in ball grinder, then ball milling 24h under 150 revs/min of rotating speed again, the sic powder after ball milling is dried;
By 300 microns of silicon-carbide particle and step(2)The carboxymethylcellulose sodium solution prepared is sufficiently mixed, in mass ratio Count carboxymethylcellulose sodium solution:Silicon-carbide particle=1:9, until carboxymethylcellulose sodium solution is in silicon-carbide particle surface shape Into one layer of uniform solution layer;
Using a small amount of multiple method by step(1)The vitrified bonding powder of middle preparation adds surface and forms carboxymethyl cellulose In the sic powder of sodium solution layer, it is stirred continuously until vitrified bonding powder is evenly coated at silicon-carbide particle surface;
Pore creating material powder is continuously added, and is stirred, pore creating material powder is distributed in the pottery for being coated on silicon-carbide particle surface Between the outside of porcelain binding agent and particle;
Pore creating material is the mixture of flake graphite in powder and activated carbon, counts flake graphite in powder in mass ratio:Activated carbon=1:1.5;
The powder of preparation is subjected to dry-pressing formed, pressure 24MPa, be supported body base substrate, and base substrate is sintered, sintering temperature Spend for 1300 degrees Celsius, be incubated 1-2h, mean porosities 38%, a diameter of 50mm, natural cooling rear supports side is 120 The non-woven fabrics base material layer that DEG C composite thickness is 700 μm can obtain compound support;
(4)The preparation of ceramic fibre transition zone
The length of first aluminium silicate fiber peacekeeping mullite fiber is trimmed to 10mm and 20mm respectively, and aluminium silicate fiber peacekeeping mullite is fine Dimension is mixed and mixed using magnetic agitation is scattered, is then added sodium cellulose glycolate and deionized water, is continued to be well mixed, so Ball milling is carried out afterwards can obtain uniform ceramic fibre transition zone slurry;
Alumina silicate fibre is counted in mass ratio:Mullite fiber:Sodium carboxymethylcellulose:Deionized water=1:1.5:1.5:65;
By ceramic fibre transition zone slurry using tape casting machine on the compound support prepared away from non-woven fabrics base material layer Side casting film-forming, obtained base film is dried in an oven, is repeated 4 times to obtain the ceramics that thickness is about 110 microns according to this Transition tunic;
(5)The preparation of filter membrane
By 25 microns of sic powder, vitrified bonding, deionized water, sodium carboxymethylcellulose is well mixed, filtered Film compound;
Sic powder is counted in mass ratio:Vitrified bonding:Deionized water:Sodium carboxymethylcellulose=10:1:4:2;
In step(4)Casting film-forming is carried out using filter membrane compound on the ceramic interlayer film surface prepared, by what is obtained 5 curtain coatings obtain the silicon carbide ceramics filter membrane that thickness is 350 microns to the drying of transition tunic repeatedly, are carried out under 1400 degrees Celsius Sinter and can obtain filter membrane after being incubated 3h.
Embodiment 3
The present embodiment provides a kind of preparation method of industrial air filter filter membrane, the preparation method of the filter membrane include with Lower step:
(1)The preparation of vitrified bonding
By water based acrylic resin, kaolin, silica sand, silica, dispersant, calcium carbonate, coupling agent, thickener and answer Rare earth is closed, is well mixed, then carries out ball milling, ball milling 33h, ball milling speed 420t/min, is put into drying baker after ball milling Dry, pulverize at 55 DEG C, you can obtain vitrified bonding powder;
Step(1)Middle vitrified bonding includes following components according to the mass fraction:
Water based acrylic resin:35 parts, kaolin:22 parts, silica sand:10-15 parts, silica:12 parts, dispersant:6 Part, calcium carbonate:2 parts, coupling agent:5 parts, thickener:4 parts, compound rare-earth:0.2 part;
Compound rare-earth includes following component by weight percentage:Y:13%, Sc:16%, Gd:9%, Sm:18%, Pr:9%, surplus is La, above each component sum are 100%;
Coupling agent is silane coupler;Dispersant is calgon;Thickener is alumina silicate;
The preparation method of water based acrylic resin is:
N-butanol is added into the three-necked flask equipped with agitator agent water-bath, is heated up to 93 DEG C, then by benzoyl peroxide Methyl methacrylate, hydroxy-ethyl acrylate, the mixed liquor of acryloid lauryl mercaptan are dissolved in, and mixed liquor is added dropwise into three In mouth flask, dropwise addition maintains 3h completions, and controls temperature after being added dropwise and being incubated 1.5h, to add benzoyl peroxide at 92 DEG C Formyl is simultaneously warming up to 105 DEG C, insulation 0.8h, and then to 39 DEG C triethylamine is added dropwise, to 7.5, heating subtracts regulation pH value in slow cooling Pressure-off removes partial solvent, finally, adds water dilution and obtains water based acrylic resin;
(2)The preparation of carboxymethylcellulose sodium solution
Sodium carboxymethylcellulose powder is put into container, deionized water is added, boils under magnetic stirring, until obtaining dense Spend the carboxymethylcellulose sodium solution for 2wt%;
(3)The preparation of compound support
Carborundum is calcined at 900 DEG C, 2.5h is then soaked in hydrogen peroxide solution, rear screening and choosing is rinsed in taking-up well Take 300 microns of silicon-carbide particle;
Sic powder is pre-processed, by sic powder, aluminum oxide abrading-ball and water in mass ratio 1:1:1.5 ratio adds Enter in ball grinder, then ball milling 22h under 145 revs/min of rotating speed again, the sic powder after ball milling is dried;
By 300 microns of silicon-carbide particle and step(2)The carboxymethylcellulose sodium solution prepared is sufficiently mixed, in mass ratio Count carboxymethylcellulose sodium solution:Silicon-carbide particle=1:8, until carboxymethylcellulose sodium solution is in silicon-carbide particle surface shape Into one layer of uniform solution layer;
Using a small amount of multiple method by step(1)The vitrified bonding powder of middle preparation adds surface and forms carboxymethyl cellulose In the sic powder of sodium solution layer, it is stirred continuously until vitrified bonding powder is evenly coated at silicon-carbide particle surface;
Pore creating material powder is continuously added, and is stirred, pore creating material powder is distributed in the pottery for being coated on silicon-carbide particle surface Between the outside of porcelain binding agent and particle;
Pore creating material is the mixture of flake graphite in powder and activated carbon, counts flake graphite in powder in mass ratio:Activated carbon=1:1.5;
The powder of preparation is subjected to dry-pressing formed, pressure 22MPa, be supported body base substrate, and base substrate is sintered, sintering temperature Spend for 1250 degrees Celsius, be incubated 1.5h, mean porosities 36%, a diameter of 45mm, natural cooling rear supports side is 110 The non-woven fabrics base material layer that DEG C composite thickness is 600 μm can obtain compound support;
(4)The preparation of ceramic fibre transition zone
The length of first aluminium silicate fiber peacekeeping mullite fiber is trimmed to 10mm and 20mm respectively, and aluminium silicate fiber peacekeeping mullite is fine Dimension is mixed and mixed using magnetic agitation is scattered, is then added sodium cellulose glycolate and deionized water, is continued to be well mixed, so Ball milling is carried out afterwards can obtain uniform ceramic fibre transition zone slurry;
Alumina silicate fibre is counted in mass ratio:Mullite fiber:Sodium carboxymethylcellulose:Deionized water=1:1.5:1.5:65;
By ceramic fibre transition zone slurry using tape casting machine on the compound support prepared away from non-woven fabrics base material layer Side casting film-forming, obtained base film is dried in an oven, is repeated 3 times to obtain the ceramics that thickness is about 105 microns according to this Transition tunic;
(5)The preparation of filter membrane
By 23 microns of sic powder, vitrified bonding, deionized water, sodium carboxymethylcellulose is well mixed, filtered Film compound;
Sic powder is counted in mass ratio:Vitrified bonding:Deionized water:Sodium carboxymethylcellulose=10:1:4:2;
In step(4)Casting film-forming is carried out using filter membrane compound on the ceramic interlayer film surface prepared, by what is obtained 4 curtain coatings obtain the silicon carbide ceramics filter membrane that thickness is 320 microns to the drying of transition tunic repeatedly, are carried out under 1350 degrees Celsius Sinter and be incubated 2h;
Configuration concentration is 4mg/ml graphene oxide solution, using press filtration mode by graphene oxide solution along perpendicular to step (5)The direction of the filter membrane prepared is permeated in the micropore of the surface of filter membrane and filter membrane;
And reaction 8h is carried out under an inert atmosphere using sodium borohydride or hydroiodic acid, obtains composite filtering film at 900 DEG C.
In the present embodiment 1-3 alumina silicate fibre is strictly controlled when preparing ceramic fibre transition zone:Mullite fiber:Carboxylic first Base sodium cellulosate:The proportioning of deionized water, the application select and count alumina silicate fibre in mass ratio:Mullite fiber:Carboxymethyl is fine Tie up plain sodium:Deionized water=1:1.5:1.5:65, wherein, the dosage of mullite fiber can influence final quality problems, with not Carry out the increasing flesh of mineral wool content, the middle Undertaking effect of ceramic fibre transition zone strengthens therewith, the uniform globality of filter membrane Become more uniform, completely, reason is that the thickness for the netted bridge formation that mullite fiber is formed increases when the training of mullite fiber content adds Add, the netted hole compact asked, prevent table and the broken space into supporter of carbonization become strong, mullite fiber added Amount, formation ceramic fibre transition region thickness is blocked up, causes filter membrane, fiber transition zone not close, appearance Nian Jie with supporter three Easy to fall off, the bending strength of filter membrane is poor, and it is that 1.5 each convenience are all carried out most preferably to choose dosage, ensures final quality.
The preparation method of the industrial air filter filter membrane of the present invention, the preparation method is simple and easy, preparation technology With very high antifalsification, the filter membrane even structure prepared, there is good high temperature resistant, high pressure and chemical stability, Filtration pressure is reduced, and is increased the service life, and filtering accuracy is high, and porosity is high, and air permeance resistance is small, uniform pore diameter, cleaning and regeneration Convenient, repeatedly curtain coating ensures the thickness of filter membrane repeatedly, and also make it that filtering film thickness selectivity is higher.
In addition to the implementation, the present invention can also have other embodiment.It is all to use equivalent substitution or equivalent transformation shape Into technical scheme, all fall within the protection domains of application claims.

Claims (8)

  1. A kind of 1. preparation method of industrial air filter filter membrane, it is characterised in that:The preparation method of the filter membrane includes Following steps:
    (1)The preparation of vitrified bonding
    By water based acrylic resin, kaolin, silica sand, silica, dispersant, calcium carbonate, coupling agent, thickener and answer Rare earth is closed, is well mixed, then carries out ball milling, ball milling 30-35h, ball milling speed 400-450t/min, is put into drying after ball milling Dry, pulverize at 50-60 DEG C in case, you can obtain vitrified bonding powder;
    (2)The preparation of carboxymethylcellulose sodium solution
    Sodium carboxymethylcellulose powder is put into container, deionized water is added, boils under magnetic stirring, until obtaining dense Spend the carboxymethylcellulose sodium solution for 2wt%;
    (3)The preparation of compound support
    Carborundum is calcined at 800-1000 DEG C, 2-3h is then soaked in hydrogen peroxide solution, after taking-up is rinsed well 300 microns of silicon-carbide particle is chosen in screening;
    By 300 microns of silicon-carbide particle and step(2)The carboxymethylcellulose sodium solution prepared is sufficiently mixed, in mass ratio Count carboxymethylcellulose sodium solution:Silicon-carbide particle=1:7-9, until carboxymethylcellulose sodium solution is on silicon-carbide particle surface Form one layer of uniform solution layer;
    Using a small amount of multiple method by step(1)The vitrified bonding powder of middle preparation adds surface and forms carboxymethyl cellulose In the sic powder of sodium solution layer, it is stirred continuously until vitrified bonding powder is evenly coated at silicon-carbide particle surface;
    Pore creating material powder is continuously added, and is stirred, pore creating material powder is distributed in the pottery for being coated on silicon-carbide particle surface Between the outside of porcelain binding agent and particle;
    The powder of preparation is subjected to dry-pressing formed, pressure 20-24MPa, be supported body base substrate, and base substrate is sintered, and is burnt Junction temperature is 1200-1300 degrees Celsius, is incubated 1-2h, mean porosities 35-38%, a diameter of 40-50mm, after natural cooling Supporter side can obtain compound support in 100-120 DEG C of compound nonwoven cloth substrate layer;
    (4)The preparation of ceramic fibre transition zone
    Aluminium silicate fiber peacekeeping mullite fiber is mixed and uses magnetic agitation is scattered to mix, then adds sodium cellulose glycolate And deionized water, continue to be well mixed, then carry out ball milling and can obtain uniform ceramic fibre transition zone slurry;
    Alumina silicate fibre is counted in mass ratio:Mullite fiber:Sodium carboxymethylcellulose:Deionized water=1:1.5:1.5:65;
    By ceramic fibre transition zone slurry using tape casting machine on the compound support prepared away from non-woven fabrics base material layer Side casting film-forming, obtained base film is dried in an oven, it is about 100-110 microns that repeatedly 3-4 times, which obtains thickness, according to this Ceramic interlayer film;
    (5)The preparation of filter membrane
    By the sic powder, vitrified bonding, deionized water of 20-25 microns, sodium carboxymethylcellulose is well mixed, obtained Filter membrane compound;
    Sic powder is counted in mass ratio:Vitrified bonding:Deionized water:Sodium carboxymethylcellulose=10:1:4:2;
    In step(4)Casting film-forming is carried out using filter membrane compound on the ceramic interlayer film surface prepared, by what is obtained 3-5 curtain coating obtains the silicon carbide ceramics filter membrane that thickness is 300-350 microns to the drying of transition tunic repeatedly, in 1300-1400 It is sintered under degree Celsius and can obtain filter membrane after being incubated 2-3h.
  2. 2. the preparation method of industrial air filter filter membrane according to claim 1, it is characterised in that:Described mistake Filter membrane is compound with graphene, and concrete operations are:
    Configuration concentration is 0.005-8mg/ml graphene oxide solution, using press filtration mode by graphene oxide solution along vertically In the step(5)The direction of the filter membrane prepared is permeated in the micropore of the surface of filter membrane and filter membrane;
    And reaction 5-10h is carried out under an inert atmosphere using sodium borohydride or hydroiodic acid, obtains combined filtration at 700-1200 DEG C Film.
  3. 3. the preparation method of industrial air filter filter membrane according to claim 1, it is characterised in that:Step(1) Described in vitrified bonding include following components according to the mass fraction:
    Water based acrylic resin:30-40 parts, kaolin:20-25 parts, silica sand:10-15 parts, silica:10-13 parts, Dispersant:5-7 parts, calcium carbonate:1-3 parts, coupling agent:4-6 parts, thickener:3-5 parts, compound rare-earth:0.1-0.3 parts;
    Described compound rare-earth includes following component by weight percentage:Y:13%, Sc:16%, Gd:9%, Sm:18%, Pr:9%, it is remaining It is 100% to measure as La, above each component sum;
    Described coupling agent is at least one of silane coupler or zirconium class coupling agent;The dispersant is calgon; Described thickener is bentonite, attapulgite or alumina silicate.
  4. 4. the preparation method of the industrial air filter filter membrane according to claim 1 or 3, it is characterised in that:It is described The preparation method of water based acrylic resin is:
    N-butanol is added into the three-necked flask equipped with agitator agent water-bath, is heated up to 90-95 DEG C, then by benzoyl peroxide first Acyl is dissolved in methyl methacrylate, hydroxy-ethyl acrylate, the mixed liquor of acryloid lauryl mercaptan, and by mixed liquor be added dropwise into In three-necked flask, dropwise addition maintains 3-4h completions, and controls temperature after being added dropwise and being incubated 1-2h, to be added at 90-95 DEG C BP is simultaneously warming up to 100-110 DEG C, insulation 0.5-1h, and then triethylamine, regulation is added dropwise to 35-45 DEG C in slow cooling PH value heats removed under reduced pressure partial solvent, finally, adds water dilution and obtain water based acrylic resin to 7.5-8.
  5. 5. the preparation method of industrial air filter filter membrane according to claim 1, it is characterised in that:Step(3) 300 microns after screening of sic powder is pre-processed, by sic powder, aluminum oxide abrading-ball and water in mass ratio 1:1: 1.5 ratio is added in ball grinder, then ball milling 20-24h under 140-150 revs/min of rotating speed again, by the carborundum powder after ball milling Expect drying, screening obtains 300 microns of carborundum.
  6. 6. the preparation method of industrial air filter filter membrane according to claim 1, it is characterised in that:The nonwoven The thickness of cloth base material layer is 500-700 μm.
  7. 7. the preparation method of industrial air filter filter membrane according to claim 1, it is characterised in that:Step(3) Described in pore creating material be the mixture of flake graphite in powder and activated carbon, count flake graphite in powder in mass ratio:Activated carbon=1:1.5.
  8. 8. the preparation method of industrial air filter filter membrane according to claim 1, it is characterised in that:Step(4) In the length of aluminium silicate fiber peacekeeping mullite fiber be trimmed to 10mm and 20mm respectively.
CN201710992280.2A 2017-10-23 2017-10-23 A kind of preparation method of industrial air filter filter membrane Withdrawn CN107511077A (en)

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CN106076256A (en) * 2016-07-06 2016-11-09 中山大学 A kind of preparation method and applications of nanometer Fe (0) porous mud material with carbon element
CN108164282A (en) * 2018-01-10 2018-06-15 淮阴师范学院 A kind of attapulgite composite ceramics film support and its preparation method and application
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
CN109603359A (en) * 2019-02-12 2019-04-12 合肥俄弈电器有限公司 A kind of high-performance filtration film for Industrial Boiler dedusting
CN109603401A (en) * 2019-02-12 2019-04-12 合肥俄弈电器有限公司 A kind of cleaner high-efficient, clean-up effect is strong
CN109999570A (en) * 2019-04-13 2019-07-12 瑞德纳米科技(广州)有限公司 A kind of preparation method of air filting material
CN110124526A (en) * 2019-04-30 2019-08-16 湖北工业大学 A kind of production method of silicon carbide inorganic ceramic membrane
CN115059806A (en) * 2022-06-27 2022-09-16 青岛优派普环保科技股份有限公司 PE pipe for fuel gas and preparation method thereof
CN115403357A (en) * 2022-08-23 2022-11-29 南京水凝科技有限公司 Underwater super-oleophobic bionic ceramic matrix and preparation method thereof
CN116040671A (en) * 2022-12-28 2023-05-02 广西华纳新材料股份有限公司 Preparation method of flaky calcium carbonate

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CN101954246A (en) * 2010-08-27 2011-01-26 清华大学 Double-layer asymmetrical surface film of porous ceramic filter tube for dust filter and preparation method thereof
CN103113110A (en) * 2012-12-04 2013-05-22 海南大学 Application method of composite silicon carbide ceramic fiber transition layer
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Cited By (16)

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Publication number Priority date Publication date Assignee Title
CN106076256A (en) * 2016-07-06 2016-11-09 中山大学 A kind of preparation method and applications of nanometer Fe (0) porous mud material with carbon element
CN108164282A (en) * 2018-01-10 2018-06-15 淮阴师范学院 A kind of attapulgite composite ceramics film support and its preparation method and application
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
CN109603359B (en) * 2019-02-12 2021-08-13 西安能度能源技术有限公司 High-performance filtering membrane for industrial boiler dust removal
CN109603359A (en) * 2019-02-12 2019-04-12 合肥俄弈电器有限公司 A kind of high-performance filtration film for Industrial Boiler dedusting
CN109603401A (en) * 2019-02-12 2019-04-12 合肥俄弈电器有限公司 A kind of cleaner high-efficient, clean-up effect is strong
CN109999570B (en) * 2019-04-13 2021-11-26 山东奥博环保科技有限公司 Preparation method of air filtering material
CN109999570A (en) * 2019-04-13 2019-07-12 瑞德纳米科技(广州)有限公司 A kind of preparation method of air filting material
CN110124526A (en) * 2019-04-30 2019-08-16 湖北工业大学 A kind of production method of silicon carbide inorganic ceramic membrane
CN110124526B (en) * 2019-04-30 2022-06-28 湖北工业大学 Production method of silicon carbide inorganic ceramic membrane
CN115059806A (en) * 2022-06-27 2022-09-16 青岛优派普环保科技股份有限公司 PE pipe for fuel gas and preparation method thereof
CN115059806B (en) * 2022-06-27 2024-02-09 青岛优派普环保科技股份有限公司 PE pipe for fuel gas and preparation method thereof
CN115403357A (en) * 2022-08-23 2022-11-29 南京水凝科技有限公司 Underwater super-oleophobic bionic ceramic matrix and preparation method thereof
CN115403357B (en) * 2022-08-23 2023-01-31 南京水凝科技有限公司 Underwater super-oleophobic bionic ceramic substrate and preparation method thereof
CN116040671A (en) * 2022-12-28 2023-05-02 广西华纳新材料股份有限公司 Preparation method of flaky calcium carbonate
CN116040671B (en) * 2022-12-28 2024-05-03 广西华纳新材料股份有限公司 Preparation method of flaky calcium carbonate

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Application publication date: 20171226