CN108218464A - A kind of preparation method of environment-friendly ceramic microfiltration membranes - Google Patents

A kind of preparation method of environment-friendly ceramic microfiltration membranes Download PDF

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CN108218464A
CN108218464A CN201810243159.4A CN201810243159A CN108218464A CN 108218464 A CN108218464 A CN 108218464A CN 201810243159 A CN201810243159 A CN 201810243159A CN 108218464 A CN108218464 A CN 108218464A
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microfiltration membranes
preparation
environment
temperature
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何敬堂
庞婉青
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Foshan Xihua Science And Technology Co Ltd
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Abstract

The present invention provides a kind of preparation methods of environment-friendly ceramic microfiltration membranes, include the following steps：By polyvinylpyrrolidone and deionized water mixed dissolution, add in cordierite powder, modified clay and microcrystalline cellulose, ball milling and obtain mixed slurry；Polyacrylic acid is added dropwise, adjusts pH value, stirring；It is slowly added to boehmite sol and Aluminum sol stirring；Wet cake is taken out and dried by fast dewatering；Grinding is granulated, and sieving takes powder；Powder is dry-pressing formed, isostatic pressing；Calcine to obtain supporter；Cordierite powder, modified clay and boehmite sol, Aluminum sol are mixed into obtain suspension；Sodium Polyacrylate, polyvinylpyrrolidone and deionized water mixed dissolution are added in suspension, evaporation is quantitative, and vacuum defoaming obtains coating liquid；Supporter is impregnated in coating liquid, is sintered after dry, natural cooling.For the average pore size of microfiltration membranes prepared by this method between 0.280 0.283 μm, pure water flux is high, has extraordinary rejection effect.

Description

A kind of preparation method of environment-friendly ceramic microfiltration membranes
Technical field
The present invention relates to a kind of preparation methods of environment-friendly ceramic microfiltration membranes.
Background technology
Inorganic ceramic membrane is since with high temperature resistant, chemical stability is good, high mechanical strength, aperture is controllable, pollution is small and makes The advantages of being lacked with organic polymer films such as long lifespans, becomes increasingly widespread to attract attention.Porous composite ceramic film usually by The multi-layer compound structure that separating layer and supporter are formed is formed, and wherein supporter assigns ceramic film-strength, and separating layer determines The separating property of film.At present, the material for preparing ceramic membrane mainly includes Al2O3, TiO2, ZrO2Deng, but this based ceramic film raw material valency Lattice are expensive, thus partly cause film manufacture of high cost, limit the further genralrlization application of ceramic membrane.In recent years, it makes pottery to reduce Porcelain film manufactures cost, and research prepares ceramic membrane using cheap raw mineral materials such as clay, zeolite, cordierite, apatite etc. becomes heat One of point.Meanwhile the pure water flux for further improving microfiltration membranes also becomes the hot spot of research.
Invention content
Technical problems to be solved：The object of the present invention is to provide a kind of preparation method of environment-friendly ceramic microfiltration membranes, institutes For the average pore size of the microfiltration membranes of preparation between 0.280-0.283 μm μm, pure water flux is high, has extraordinary rejection effect.
Technical solution：A kind of preparation method of environment-friendly ceramic microfiltration membranes, ingredient by weight, include the following steps：
(1) mixed dissolution under 85 DEG C of water-bath by 1-2 parts of polyvinylpyrrolidones and 100-150 parts of deionized waters moves into ball In grinding jar, add in 100-120 parts of cordierite powder, 10-12 parts of modified clays and 8-10 parts of microcrystalline celluloses, ball milling 30-50min and obtain Mixed slurry；
(2) 0.8-1 parts of polyacrylic acid are added dropwise, and the pH value for adjusting mixed slurry continues to stir 30-40min to 4-5；
(3) it is transferred in stirring container, with vigorous stirring, is slowly added to 2-5 parts of boehmite sols and 2-4 parts of Aluminum sols, stirs Mix 2-3h；
(4) it pours into and fast dewatering is carried out in dry plaster mold, wet cake is taken out, be placed in 60-65 DEG C of drying box and dry, control Moisture content processed is between 4%-7%；
(5) it is ground and is granulated after taking out, cross 80 mesh and 40 mesh sieve, sieve takes the powder between 40-80 mesh；
(6) powder under 15-20MPa is carried out dry-pressing formed, obtains disc-shaped green compact sample, green compact are carried out under 150MPa Isostatic pressing；
(7) green compact after isostatic pressing to be calcined, be warming up to 500 DEG C and keep the temperature 1h, heating rate is 2 DEG C/min, after Continuous to be warming up to 1000 DEG C and keep the temperature 30min, heating rate is 5 DEG C/min, is continuously heating to 1450-1600 and keeps the temperature 2h, is heated up Rate is 10 DEG C/min, finally with stove natural cooling, obtains supporter；
(8) 10-25 parts of cordierite powder, 1-1.5 parts of modified clays and 30-50 parts of boehmite sols, 20-40 parts of Aluminum sols are mixed It closes, is vigorously stirred, obtains suspension；
(9) by 0.5-1 parts of Sodium Polyacrylates, 2-4 parts of polyvinylpyrrolidones and 50-70 parts of deionized waters under 85 DEG C of water-bath Mixed dissolution is slowly added in suspension, and quantification of 100 parts of evaporation is vigorously stirred in 70 DEG C of water-bath, carries out vacuum defoaming 1h obtains uniform coating liquid；
(10) supporter is impregnated in coating liquid, time of immersion 10-35s is carried out after spontaneously drying 12h after taking-up at room temperature Sintering, is warming up to 500 DEG C and keeps the temperature 1h, and heating rate is 2 DEG C/min, is continuously heating to 1000-1300 DEG C and keeps the temperature 2-4h, rises Warm rate is 5 DEG C/min, finally with stove natural cooling.
It is further preferred that the preparation method of the modified clay is：
The first step：By 1-3 parts of dodecyl sodium sulfates and 1-3 parts of Cetyltrimethylammonium bromides and 10-20 parts of deionized waters, 20-30min is mixed；
Second step：1-3 parts of clays are added in, stir 10-20min；
Third walks：Filtering, drying.
It is further preferred that the grain size of cordierite powder and modified clay is 10-15 μm in the step (1).
It is further preferred that the disc-shaped green compact sample size is Φ 45mm × 3mm.
It is further preferred that the grain size of cordierite powder and modified clay is 80-100nm in the step (8).
It is further preferred that in the boehmite sol boehmite a concentration of 1.5-2.0wt%.
It is further preferred that the pH value of the Aluminum sol is 6.7.
Advantageous effect：
1. by adjusting sol pH, make its surface positively charged, by adjusting the pH value of slurry, make its negatively charged.Pass through Electrostatic adsorption makes nano level micelle be uniformly coated on pulp particle surface, and pass through the addition for controlling colloidal sol and Firing degree, it can be achieved that prepare the supporter of high porosity, high intensity, good corrosion resistance at low temperature.
2. improve the film forming of coating liquid by introducing colloidal sol simultaneously in coating liquid with Sodium Polyacrylate, polyvinylpyrrolidone Performance.
3. the effect of being cross-linked with each other can be generated between colloidal sol, Sodium Polyacrylate and polyvinylpyrrolidone and is generated huge Colloid network structure enables ceramic micro filter film to resist the capillarity attraction effect of support body opening to a certain extent, so as to subtract Film forming particle infiltration enters in supporter and causes the blocking in hole less, is prepared in macropore supporting body surface so as to directly micro- Filter membrane.
Specific embodiment
Embodiment 1
A kind of preparation method of environment-friendly ceramic microfiltration membranes, ingredient by weight, include the following steps：
(1) mixed dissolution under 85 DEG C of water-bath by 1 part of polyvinylpyrrolidone and 100 parts of deionized waters is moved into ball grinder, It adds in 100 parts of cordierite powder, 10 parts of modified clays and 8 parts of microcrystalline celluloses, ball milling 30min and obtains mixed slurry；
(2) 0.8 part of polyacrylic acid is added dropwise, and the pH value for adjusting mixed slurry continues to stir 30min to 4；
(3) it is transferred in stirring container, with vigorous stirring, is slowly added to 2 parts of boehmite sols and 2 parts of Aluminum sols, stirs 2h；
(4) it pours into and fast dewatering is carried out in dry plaster mold, wet cake is taken out, be placed in 60 DEG C of drying boxes and dry, control Moisture content is 4%；
(5) it is ground and is granulated after taking out, cross 80 mesh and 40 mesh sieve, sieve takes the powder between 40-80 mesh；
(6) powder under 15MPa is carried out dry-pressing formed, obtains disc-shaped green compact sample, green compact are carried out under 150MPa etc. Hydrostatic profile；
(7) green compact after isostatic pressing to be calcined, be warming up to 500 DEG C and keep the temperature 1h, heating rate is 2 DEG C/min, after Continuous to be warming up to 1000 DEG C and keep the temperature 30min, heating rate is 5 DEG C/min, is continuously heating to 1450 DEG C and keeps the temperature 2h, heating rate For 10 DEG C/min, finally with stove natural cooling, supporter is obtained；
(8) 10 parts of cordierite powder, 1 part of modified clay and 30 parts of boehmite sols, 20 parts of Aluminum sols are mixed, is vigorously stirred, obtains Suspension；
(9) 0.5 part of Sodium Polyacrylate, 2 parts of polyvinylpyrrolidones and 50 parts of deionized waters are mixed under 85 DEG C of water-bath molten Solution, is slowly added in suspension, and quantification of 100 parts of evaporation is vigorously stirred in 70 DEG C of water-bath, carries out vacuum defoaming 1h, obtains Uniform coating liquid；
(10) supporter is impregnated in coating liquid, time of immersion 10s is burnt after spontaneously drying 12h at room temperature after taking-up Knot, is warming up to 500 DEG C and keeps the temperature 1h, and heating rate is 2 DEG C/min, is continuously heating to 1000 DEG C and keeps the temperature 2h, heating rate 5 DEG C/min, finally with stove natural cooling.
Embodiment 2
A kind of preparation method of environment-friendly ceramic microfiltration membranes, ingredient by weight, include the following steps：
(1) mixed dissolution under 85 DEG C of water-bath by 1.5 parts of polyvinylpyrrolidones and 120 parts of deionized waters moves into ball grinder In, it adds in 110 parts of cordierite powder, 11 parts of modified clays and 9 parts of microcrystalline celluloses, ball milling 35min and obtains mixed slurry；
(2) 0.9 part of polyacrylic acid is added dropwise, and the pH value for adjusting mixed slurry continues to stir 35min to 4.5；
(3) it is transferred in stirring container, with vigorous stirring, is slowly added to 3 parts of boehmite sols and 3 parts of Aluminum sols, stir 2.5h；
(4) it pours into and fast dewatering is carried out in dry plaster mold, wet cake is taken out, be placed in 62 DEG C of drying boxes and dry, control Moisture content is 5%；
(5) it is ground and is granulated after taking out, cross 80 mesh and 40 mesh sieve, sieve takes the powder between 40-80 mesh；
(6) powder under 17MPa is carried out dry-pressing formed, obtains disc-shaped green compact sample, green compact are carried out under 150MPa etc. Hydrostatic profile；
(7) green compact after isostatic pressing to be calcined, be warming up to 500 DEG C and keep the temperature 1h, heating rate is 2 DEG C/min, after Continuous to be warming up to 1000 DEG C and keep the temperature 30min, heating rate is 5 DEG C/min, is continuously heating to 1500 and keeps the temperature 2h, heating rate is 10 DEG C/min, finally with stove natural cooling, obtain supporter；
(8) 15 parts of cordierite powder, 1.2 parts of modified clays and 35 parts of boehmite sols, 25 parts of Aluminum sols are mixed, are vigorously stirred, Obtain suspension；
(9) 0.7 part of Sodium Polyacrylate, 3 parts of polyvinylpyrrolidones and 55 parts of deionized waters are mixed under 85 DEG C of water-bath molten Solution, is slowly added in suspension, and quantification of 100 parts of evaporation is vigorously stirred in 70 DEG C of water-bath, carries out vacuum defoaming 1h, obtains Uniform coating liquid；
(10) supporter is impregnated in coating liquid, time of immersion 15s is burnt after spontaneously drying 12h at room temperature after taking-up Knot, is warming up to 500 DEG C and keeps the temperature 1h, and heating rate is 2 DEG C/min, is continuously heating to 1100 DEG C and keeps the temperature 3h, heating rate 5 DEG C/min, finally with stove natural cooling.
Embodiment 3
A kind of preparation method of environment-friendly ceramic microfiltration membranes, ingredient by weight, include the following steps：
(1) mixed dissolution under 85 DEG C of water-bath by 1.5 parts of polyvinylpyrrolidones and 130 parts of deionized waters moves into ball grinder In, it adds in 110 parts of cordierite powder, 11 parts of modified clays and 9 parts of microcrystalline celluloses, ball milling 40min and obtains mixed slurry；
(2) 0.9 part of polyacrylic acid is added dropwise, and the pH value for adjusting mixed slurry continues to stir 35min to 4.5；
(3) it is transferred in stirring container, with vigorous stirring, is slowly added to 4 parts of boehmite sols and 3 parts of Aluminum sols, stir 2.5h；
(4) it pours into and fast dewatering is carried out in dry plaster mold, wet cake is taken out, be placed in 63 DEG C of drying boxes and dry, control Moisture content is 6%；
(5) it is ground and is granulated after taking out, cross 80 mesh and 40 mesh sieve, sieve takes the powder between 40-80 mesh；
(6) powder under 18MPa is carried out dry-pressing formed, obtains disc-shaped green compact sample, green compact are carried out under 150MPa etc. Hydrostatic profile；
(7) green compact after isostatic pressing to be calcined, be warming up to 500 DEG C and keep the temperature 1h, heating rate is 2 DEG C/min, after Continuous to be warming up to 1000 DEG C and keep the temperature 30min, heating rate is 5 DEG C/min, is continuously heating to 1550 and keeps the temperature 2h, heating rate is 10 DEG C/min, finally with stove natural cooling, obtain supporter；
(8) 20 parts of cordierite powder, 1.3 parts of modified clays and 40 parts of boehmite sols, 30 parts of Aluminum sols are mixed, are vigorously stirred, Obtain suspension；
(9) 0.8 part of Sodium Polyacrylate, 3 parts of polyvinylpyrrolidones and 60 parts of deionized waters are mixed under 85 DEG C of water-bath molten Solution, is slowly added in suspension, and quantification of 100 parts of evaporation is vigorously stirred in 70 DEG C of water-bath, carries out vacuum defoaming 1h, obtains Uniform coating liquid；
(10) supporter is impregnated in coating liquid, time of immersion 25s is burnt after spontaneously drying 12h at room temperature after taking-up Knot, is warming up to 500 DEG C and keeps the temperature 1h, and heating rate is 2 DEG C/min, is continuously heating to 1200 DEG C and keeps the temperature 3h, heating rate 5 DEG C/min, finally with stove natural cooling.
Embodiment 4
A kind of preparation method of environment-friendly ceramic microfiltration membranes, ingredient by weight, include the following steps：
(1) mixed dissolution under 85 DEG C of water-bath by 2 parts of polyvinylpyrrolidones and 150 parts of deionized waters is moved into ball grinder, It adds in 120 parts of cordierite powder, 12 parts of modified clays and 10 parts of microcrystalline celluloses, ball milling 50min and obtains mixed slurry；
(2) 1 part of polyacrylic acid is added dropwise, and the pH value for adjusting mixed slurry continues to stir 40min to 5；
(3) it is transferred in stirring container, with vigorous stirring, is slowly added to 5 parts of boehmite sols and 4 parts of Aluminum sols, stirs 3h；
(4) it pours into and fast dewatering is carried out in dry plaster mold, wet cake is taken out, be placed in 65 DEG C of drying boxes and dry, control Moisture content is 7%；
(5) it is ground and is granulated after taking out, cross 80 mesh and 40 mesh sieve, sieve takes the powder between 40-80 mesh；
(6) powder under 20MPa is carried out dry-pressing formed, obtains disc-shaped green compact sample, green compact are carried out under 150MPa etc. Hydrostatic profile；
(7) green compact after isostatic pressing to be calcined, be warming up to 500 DEG C and keep the temperature 1h, heating rate is 2 DEG C/min, after Continuous to be warming up to 1000 DEG C and keep the temperature 30min, heating rate is 5 DEG C/min, is continuously heating to 1600 and keeps the temperature 2h, heating rate is 10 DEG C/min, finally with stove natural cooling, obtain supporter；
(8) 25 parts of cordierite powder, 1.5 parts of modified clays and 50 parts of boehmite sols, 40 parts of Aluminum sols are mixed, are vigorously stirred, Obtain suspension；
(9) by 1 part of Sodium Polyacrylate, 4 parts of polyvinylpyrrolidones and 70 parts of deionized waters mixed dissolution under 85 DEG C of water-bath, It is slowly added in suspension, quantification of 100 parts of evaporation is vigorously stirred in 70 DEG C of water-bath, carry out vacuum defoaming 1h, obtain Even coating liquid；
(10) supporter is impregnated in coating liquid, time of immersion 35s is burnt after spontaneously drying 12h at room temperature after taking-up Knot, is warming up to 500 DEG C and keeps the temperature 1h, and heating rate is 2 DEG C/min, is continuously heating to 1300 DEG C and keeps the temperature 4h, heating rate 5 DEG C/min, finally with stove natural cooling.
Comparative example 1
The present embodiment is with embodiment 1 the difference is that replacing modified clay with cordierite powder, specially：
A kind of preparation method of environment-friendly ceramic microfiltration membranes, ingredient by weight, include the following steps：
(1) mixed dissolution under 85 DEG C of water-bath by 1 part of polyvinylpyrrolidone and 100 parts of deionized waters is moved into ball grinder, It adds in 110 parts of cordierite powder and 8 parts of microcrystalline celluloses, ball milling 30min obtains mixed slurry；
(2) 0.8 part of polyacrylic acid is added dropwise, and the pH value for adjusting mixed slurry continues to stir 30min to 4；
(3) it is transferred in stirring container, with vigorous stirring, is slowly added to 2 parts of boehmite sols and 2 parts of Aluminum sols, stirs 2h；
(4) it pours into and fast dewatering is carried out in dry plaster mold, wet cake is taken out, be placed in 60 DEG C of drying boxes and dry, control Moisture content is 4%；
(5) it is ground and is granulated after taking out, cross 80 mesh and 40 mesh sieve, sieve takes the powder between 40-80 mesh；
(6) powder under 15MPa is carried out dry-pressing formed, obtains disc-shaped green compact sample, green compact are carried out under 150MPa etc. Hydrostatic profile；
(7) green compact after isostatic pressing to be calcined, be warming up to 500 DEG C and keep the temperature 1h, heating rate is 2 DEG C/min, after Continuous to be warming up to 1000 DEG C and keep the temperature 30min, heating rate is 5 DEG C/min, is continuously heating to 1450 DEG C and keeps the temperature 2h, heating rate For 10 DEG C/min, finally with stove natural cooling, supporter is obtained；
(8) 11 parts of cordierite powder and 30 parts of boehmite sols, 20 parts of Aluminum sols are mixed, is vigorously stirred, obtains suspension；
(9) 0.5 part of Sodium Polyacrylate, 2 parts of polyvinylpyrrolidones and 50 parts of deionized waters are mixed under 85 DEG C of water-bath molten Solution, is slowly added in suspension, and quantification of 100 parts of evaporation is vigorously stirred in 70 DEG C of water-bath, carries out vacuum defoaming 1h, obtains Uniform coating liquid；
(10) supporter is impregnated in coating liquid, time of immersion 10s is burnt after spontaneously drying 12h at room temperature after taking-up Knot, is warming up to 500 DEG C and keeps the temperature 1h, and heating rate is 2 DEG C/min, is continuously heating to 1000 DEG C and keeps the temperature 2h, heating rate 5 DEG C/min, finally with stove natural cooling.
Comparative example 2
The present embodiment is with embodiment 1 the difference is that replacing Aluminum sol with boehmite sol, specially：
A kind of preparation method of environment-friendly ceramic microfiltration membranes, ingredient by weight, include the following steps：
(1) mixed dissolution under 85 DEG C of water-bath by 1 part of polyvinylpyrrolidone and 100 parts of deionized waters is moved into ball grinder, It adds in 100 parts of cordierite powder, 10 parts of modified clays and 8 parts of microcrystalline celluloses, ball milling 30min and obtains mixed slurry；
(2) 0.8 part of polyacrylic acid is added dropwise, and the pH value for adjusting mixed slurry continues to stir 30min to 4；
(3) it is transferred in stirring container, with vigorous stirring, is slowly added to 4 parts of boehmite sols, stirs 2h；
(4) it pours into and fast dewatering is carried out in dry plaster mold, wet cake is taken out, be placed in 60 DEG C of drying boxes and dry, control Moisture content is 4%；
(5) it is ground and is granulated after taking out, cross 80 mesh and 40 mesh sieve, sieve takes the powder between 40-80 mesh；
(6) powder under 15MPa is carried out dry-pressing formed, obtains disc-shaped green compact sample, green compact are carried out under 150MPa etc. Hydrostatic profile；
(7) green compact after isostatic pressing to be calcined, be warming up to 500 DEG C and keep the temperature 1h, heating rate is 2 DEG C/min, after Continuous to be warming up to 1000 DEG C and keep the temperature 30min, heating rate is 5 DEG C/min, is continuously heating to 1450 DEG C and keeps the temperature 2h, heating rate For 10 DEG C/min, finally with stove natural cooling, supporter is obtained；
(8) 10 parts of cordierite powder, 1 part of modified clay and 50 parts of boehmite sols are mixed, is vigorously stirred, obtains suspension；
(9) 0.5 part of Sodium Polyacrylate, 2 parts of polyvinylpyrrolidones and 50 parts of deionized waters are mixed under 85 DEG C of water-bath molten Solution, is slowly added in suspension, and quantification of 100 parts of evaporation is vigorously stirred in 70 DEG C of water-bath, carries out vacuum defoaming 1h, obtains Uniform coating liquid；
(10) supporter is impregnated in coating liquid, time of immersion 10s is burnt after spontaneously drying 12h at room temperature after taking-up Knot, is warming up to 500 DEG C and keeps the temperature 1h, and heating rate is 2 DEG C/min, is continuously heating to 1000 DEG C and keeps the temperature 2h, heating rate 5 DEG C/min, finally with stove natural cooling.
Comparative example 3
The present embodiment is with embodiment 1 the difference is that replacing Sodium Polyacrylate with polyvinylpyrrolidone, specially：
A kind of preparation method of environment-friendly ceramic microfiltration membranes, ingredient by weight, include the following steps：
(1) mixed dissolution under 85 DEG C of water-bath by 1 part of polyvinylpyrrolidone and 100 parts of deionized waters is moved into ball grinder, It adds in 100 parts of cordierite powder, 10 parts of modified clays and 8 parts of microcrystalline celluloses, ball milling 30min and obtains mixed slurry；
(2) 0.8 part of polyacrylic acid is added dropwise, and the pH value for adjusting mixed slurry continues to stir 30min to 4；
(3) it is transferred in stirring container, with vigorous stirring, is slowly added to 2 parts of boehmite sols and 2 parts of Aluminum sols, stirs 2h；
(4) it pours into and fast dewatering is carried out in dry plaster mold, wet cake is taken out, be placed in 60 DEG C of drying boxes and dry, control Moisture content is 4%；
(5) it is ground and is granulated after taking out, cross 80 mesh and 40 mesh sieve, sieve takes the powder between 40-80 mesh；
(6) powder under 15MPa is carried out dry-pressing formed, obtains disc-shaped green compact sample, green compact are carried out under 150MPa etc. Hydrostatic profile；
(7) green compact after isostatic pressing to be calcined, be warming up to 500 DEG C and keep the temperature 1h, heating rate is 2 DEG C/min, after Continuous to be warming up to 1000 DEG C and keep the temperature 30min, heating rate is 5 DEG C/min, is continuously heating to 1450 DEG C and keeps the temperature 2h, heating rate For 10 DEG C/min, finally with stove natural cooling, supporter is obtained；
(8) 10 parts of cordierite powder, 1 part of modified clay and 30 parts of boehmite sols, 20 parts of Aluminum sols are mixed, is vigorously stirred, obtains Suspension；
(9) mixed dissolution under 85 DEG C of water-bath by 2.5 parts of polyvinylpyrrolidones and 50 parts of deionized waters, is slowly added to suspend In liquid, quantification of 100 parts of evaporation is vigorously stirred in 70 DEG C of water-bath, vacuum defoaming 1h is carried out, obtains uniform coating liquid；
(10) supporter is impregnated in coating liquid, time of immersion 10s is burnt after spontaneously drying 12h at room temperature after taking-up Knot, is warming up to 500 DEG C and keeps the temperature 1h, and heating rate is 2 DEG C/min, is continuously heating to 1000 DEG C and keeps the temperature 2h, heating rate 5 DEG C/min, finally with stove natural cooling.
The partial properties index of 1 supporter of table
Name of product Average pore size (μm) Mean porosities (%) Bending strength (MPa)
Embodiment 1 4.92 52.1 37.76
Embodiment 2 4.93 52.3 37.83
Embodiment 3 4.93 52.4 37.89
Embodiment 4 4.92 52.2 37.84
The partial properties index of 2 environment-friendly ceramic microfiltration membranes of table
Name of product Average pore size (μm) Pure water flux (Lm-2·h-1·bar-1)
Embodiment 1 0.283 1380
Embodiment 2 0.281 1381
Embodiment 3 0.280 1384
Embodiment 4 0.281 1383
Comparative example 1 0.291 1351
Comparative example 2 0.251 1282
Comparative example 3 0.294 1359
The partial properties index of environment-friendly ceramic microfiltration membranes prepared by the method for the present invention is seen the above table, we can be averaged with microfiltration membranes Between 0.280-0.283 μm, pure water flux reaches as high as 1384Lm in aperture-2·h-1·bar-1, there is extraordinary section Stay effect.

Claims (7)

1. a kind of preparation method of environment-friendly ceramic microfiltration membranes, it is characterised in that：Ingredient by weight, includes the following steps：
(1) mixed dissolution under 85 DEG C of water-bath by 1-2 parts of polyvinylpyrrolidones and 100-150 parts of deionized waters moves into ball In grinding jar, add in 100-120 parts of cordierite powder, 10-12 parts of modified clays and 8-10 parts of microcrystalline celluloses, ball milling 30-50min and obtain Mixed slurry；
(2) 0.8-1 parts of polyacrylic acid are added dropwise, and the pH value for adjusting mixed slurry continues to stir 30-40min to 4-5；
(3) it is transferred in stirring container, with vigorous stirring, is slowly added to 2-5 parts of boehmite sols and 2-4 parts of Aluminum sols, stirs Mix 2-3h；
(4) it pours into and fast dewatering is carried out in dry plaster mold, wet cake is taken out, be placed in 60-65 DEG C of drying box and dry, control Moisture content processed is between 4%-7%；
(5) it is ground and is granulated after taking out, cross 80 mesh and 40 mesh sieve, sieve takes the powder between 40-80 mesh；
(6) powder under 15-20MPa is carried out dry-pressing formed, obtains disc-shaped green compact sample, green compact are carried out under 150MPa Isostatic pressing；
(7) green compact after isostatic pressing to be calcined, be warming up to 500 DEG C and keep the temperature 1h, heating rate is 2 DEG C/min, after Continuous to be warming up to 1000 DEG C and keep the temperature 30min, heating rate is 5 DEG C/min, is continuously heating to 1450-1600 and keeps the temperature 2h, is heated up Rate is 10 DEG C/min, finally with stove natural cooling, obtains supporter；
(8) 10-25 parts of cordierite powder, 1-1.5 parts of modified clays and 30-50 parts of boehmite sols, 20-40 parts of Aluminum sols are mixed It closes, is vigorously stirred, obtains suspension；
(9) by 0.5-1 parts of Sodium Polyacrylates, 2-4 parts of polyvinylpyrrolidones and 50-70 parts of deionized waters under 85 DEG C of water-bath Mixed dissolution is slowly added in suspension, and quantification of 100 parts of evaporation is vigorously stirred in 70 DEG C of water-bath, carries out vacuum defoaming 1h obtains uniform coating liquid；
(10) supporter is impregnated in coating liquid, time of immersion 10-35s is carried out after spontaneously drying 12h after taking-up at room temperature Sintering, is warming up to 500 DEG C and keeps the temperature 1h, and heating rate is 2 DEG C/min, is continuously heating to 1000-1300 DEG C and keeps the temperature 2-4h, rises Warm rate is 5 DEG C/min, finally with stove natural cooling.
2. a kind of preparation method of environment-friendly ceramic microfiltration membranes according to claim 1, it is characterised in that：The modification is glued Soil preparation method be：
The first step：By 1-3 parts of dodecyl sodium sulfates and 1-3 parts of Cetyltrimethylammonium bromides and 10-20 parts of deionized waters, 20-30min is mixed；
Second step：1-3 parts of clays are added in, stir 10-20min；
Third walks：Filtering, drying.
3. a kind of preparation method of environment-friendly ceramic microfiltration membranes according to claim 1, it is characterised in that：The step (1) grain size of cordierite powder and modified clay is 10-15 μm in.
4. a kind of preparation method of environment-friendly ceramic microfiltration membranes according to claim 1, it is characterised in that：The disc-shaped Green compact sample size is Φ 45mm × 3mm.
5. a kind of preparation method of environment-friendly ceramic microfiltration membranes according to claim 1, it is characterised in that：The step (8) grain size of cordierite powder and modified clay is 80-100nm in.
6. a kind of preparation method of environment-friendly ceramic microfiltration membranes according to claim 1, it is characterised in that：The boehmite A concentration of 1.5-2.0wt% of boehmite in colloidal sol.
7. a kind of preparation method of environment-friendly ceramic microfiltration membranes according to claim 1, it is characterised in that：The Aluminum sol PH value be 6.7.
CN201810243159.4A 2018-03-22 2018-03-22 A kind of preparation method of environment-friendly ceramic microfiltration membranes Pending CN108218464A (en)

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CN109020599A (en) * 2018-09-11 2018-12-18 刘爱 A method of preparing ceramic micro filter film
CN109516784A (en) * 2018-12-26 2019-03-26 高化学（江苏）化工新材料有限责任公司 A kind of preparation method handling catalyst production waste water microfiltration membranes
CN110256112A (en) * 2019-06-26 2019-09-20 深圳市商德先进陶瓷股份有限公司 Ceramic filter membrane and preparation method thereof
CN113121241A (en) * 2021-04-25 2021-07-16 南京依柯卡特排放技术股份有限公司 High-flux silicon carbide ceramic filter membrane and preparation method thereof
CN114345137A (en) * 2021-12-31 2022-04-15 浙江工业大学 Ceramic microfiltration membrane with black talc as inorganic film-forming powder and preparation method thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109020599A (en) * 2018-09-11 2018-12-18 刘爱 A method of preparing ceramic micro filter film
CN109516784A (en) * 2018-12-26 2019-03-26 高化学（江苏）化工新材料有限责任公司 A kind of preparation method handling catalyst production waste water microfiltration membranes
CN110256112A (en) * 2019-06-26 2019-09-20 深圳市商德先进陶瓷股份有限公司 Ceramic filter membrane and preparation method thereof
CN113121241A (en) * 2021-04-25 2021-07-16 南京依柯卡特排放技术股份有限公司 High-flux silicon carbide ceramic filter membrane and preparation method thereof
CN113121241B (en) * 2021-04-25 2022-03-22 南京依柯卡特排放技术股份有限公司 High-flux silicon carbide ceramic filter membrane and preparation method thereof
CN114345137A (en) * 2021-12-31 2022-04-15 浙江工业大学 Ceramic microfiltration membrane with black talc as inorganic film-forming powder and preparation method thereof
CN114345137B (en) * 2021-12-31 2022-11-25 浙江工业大学 Ceramic microfiltration membrane with black talc as inorganic film-forming powder and preparation method thereof

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Application publication date: 20180629