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 PDFInfo
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/54—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms
- B01D46/543—Particle separators, e.g. dust precipitators, using ultra-fine filter sheets or diaphragms using membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation 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
- B01D53/22—Separation 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
- B01D53/228—Separation 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0095—Drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
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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
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)
- 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 bondingBy 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 solutionSodium 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 supportCarborundum 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 zoneAluminium 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 membraneBy 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. 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. 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. 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. 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. 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. 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. 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.
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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 |
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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 |
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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 |
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Application publication date: 20171226 |