CN108499372A - A method of preparing high tenacity porous ceramic film support using microorganism - Google Patents
A method of preparing high tenacity porous ceramic film support using microorganism Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 86
- 238000000034 method Methods 0.000 title claims abstract description 20
- 244000005700 microbiome Species 0.000 title claims abstract description 18
- 239000012528 membrane Substances 0.000 claims abstract description 34
- 239000002002 slurry Substances 0.000 claims abstract description 27
- 244000144730 Amygdalus persica Species 0.000 claims abstract description 26
- 235000006040 Prunus persica var persica Nutrition 0.000 claims abstract description 26
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 15
- 238000001354 calcination Methods 0.000 claims abstract description 14
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 36
- 241000209094 Oryza Species 0.000 claims description 32
- 235000007164 Oryza sativa Nutrition 0.000 claims description 32
- 239000010903 husk Substances 0.000 claims description 32
- 235000009566 rice Nutrition 0.000 claims description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 25
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- 229910052786 argon Inorganic materials 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000012423 maintenance Methods 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 9
- 239000005995 Aluminium silicate Substances 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims description 8
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 claims description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 6
- 238000000855 fermentation Methods 0.000 abstract description 6
- 230000004151 fermentation Effects 0.000 abstract description 6
- 238000005253 cladding Methods 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 3
- 239000001569 carbon dioxide Substances 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract description 3
- 239000006260 foam Substances 0.000 abstract description 2
- 230000000813 microbial effect Effects 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 description 8
- 230000008023 solidification Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 5
- 239000003610 charcoal Substances 0.000 description 4
- 238000003837 high-temperature calcination Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- 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
- B01D69/10—Supported membranes; Membrane supports
-
- 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
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Immobilizing And Processing Of Enzymes And Microorganisms (AREA)
Abstract
The present invention relates to ceramic membrane preparing technical fields, and in particular to a method of preparing high tenacity porous ceramic film support using microorganism.The self-control toughening material silicon carbide whisker of the present invention, since it is with netted keel structure, so that the extraneous stress that ceramic film support is subject to is dispersed into several small parts, the present invention is also added into the sodium peroxide and biogas slurry of peach gum cladding in the preparation, and prepare ceramic film support green compact using it, it puts the green body into the greenhouse of high temperature and humidity and conserves, peach gum gradually by feeding totally, therefore the sodium peroxide of peach gum cladding is exposed, with the contact with moisture reaction in green compact, the carbon dioxide collective effect generated with microbial fermentation foams to ceramic film support green compact, to form uniform hole in green compact, final calcining molding can be obtained high tenacity porous ceramic film support, ceramic film support porosity produced by the present invention is high, pore size is uniform, toughness is strong, it has broad application prospects.
Description
Technical field
The present invention relates to ceramic membrane preparing technical fields, and in particular to a kind of to prepare high tenacity porous ceramics using microorganism
The method of film support.
Background technology
Ceramic membrane is also known as inorganic ceramic membrane, is prepared and the anisotropic membrane of formation through special process with inorganic ceramic material.
Ceramic membrane tube wall gathers micropore, and under pressure, material liquid flows in membrane tube or on the outside of film, and small-molecule substance penetrates film,
Macromolecular substances are rejected by, to reach the purpose of separation, concentration, purifying and environmental protection.Ceramic membrane has separative efficiency height, effect
Fruit is stable, chemical stability is good, acid and alkali-resistance, organic solvent-resistant, resistance to bacterium, high temperature resistant, antipollution, high mechanical strength, regenerability
Numerous advantages such as good, separation process is simple, low energy consumption, simple and convenient operation and maintenance, service life length, be successfully applied to food,
Beverage, plant（Medicine）The various fields such as object depth processing, biological medicine, fermentation, fine chemistry industry, can be used for separation in technical process,
Clarification, purifying, concentration, degerming, desalination etc..
According to the difference of supporter, the configuration of ceramic membrane can be divided into tablet, tubular type, three kinds of multichannel.Porous ceramic film can
To regard a kind of porous functionally gradient material (FGM) as, it is made of porous ceramic film support, middle layer and film layer three parts, wherein supporter
The basis of porous ceramic film preparation and application, effect be enough mechanical strengths are provided for film layer, while also will have compared with
High permeability, this suffers from important influence to the preparation of film layer and the stability in use of film.Porous ceramic film support is made
It is after being uniformly mixed molding with suitable additive by raw material, to be formed through high temperature sintering for a kind of novel ceramic material, in
The stomata largely to communicate with each other is contained in portion, but ceramic film support common at present is disadvantageous in that porosity is low,
Hole is inhomogenous, is easy to block after use, it is difficult to backwash, fouling membrane is serious, and ceramic film support brittleness is big, elasticity
It is low, influence its use scope.
Because a kind of porosity of the invention is high, aperture is uniform, and the ceramic film support that toughness is high, to ceramic film preparation skill
Art field has positive meaning.
Invention content
Present invention mainly solves the technical issues of, for common ceramic membrane at present, that there are porositys is low, hole is inhomogenous,
It is easy to block after use, it is difficult to backwash, fouling membrane is serious, and ceramic membrane brittleness is big, and elasticity is low, influences its use scope
Defect provides a kind of method preparing high tenacity porous ceramic film support using microorganism.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A method of preparing high tenacity porous ceramic film support using microorganism, it is characterised in that specifically preparation process is：
（1）It weighs rice husk deionized water to rinse 3~5 times, the rice husk after flushing is put into retort, heat preservation charing obtains
Charring rice husk is fitted into after mixing charring rice husk and iron powder in vacuum drying oven；
（2）Argon gas is passed through into above-mentioned vacuum drying oven, under protection of argon gas heat temperature raising, pyrolytic conversion handles 4~5h, is converted
Product, stopping is passed through argon gas, and reduces temperature, keeps the temperature 2~3h of oxidation processes, then oxidation product hydrofluoric acid is rinsed 3~5
Time, obtain self-control toughening silicon carbide whisker；
（3）Weigh potassium feldspar and kaolin, silica and aluminium oxide is put into togerther in ball grinder, milled processed 20~
30min obtains mixed-powder, and ceramic slurry is obtained after mixed-powder and polyvinyl alcohol and water are mixed, spare；
（4）It weighs peach gum to be put into beaker, beaker is moved into water-bath, increase water-bath pot temperature to 70~80 DEG C, insulated and stirred
20~30min continuously adds sodium peroxide into beaker, continues to be stirred 2~3h, be stirred end until peach gum fusing
Afterwards, natural cooling cures, and obtains cured product；
（5）Above-mentioned cured product is put into 20~30min of crushing in airslide disintegrating mill and obtains crushed material, by spare ceramic slurry
After material, self-control toughening silicon carbide whisker, above-mentioned cured product and biogas slurry mixing in injection stainless steel mould, it is pressed into tablet press machine
Ceramic membrane green compact；
（6）Above-mentioned ceramic membrane green compact are put into greenhouse, maintenance 2~3 days are stood, the ceramic membrane green compact after maintenance are moved into high temperature
In calcining furnace, 200 DEG C first are warming up to the rate of 5 DEG C/min, keeps the temperature 30~35min, then heat up with the rate program of 3 DEG C/min
To 1300 DEG C, heat preservation 2~4h of calcining, natural cooling discharging is to get high tenacity porous ceramic film support after calcining.
Step（1）Described in heat preservation charing temperature be 400~500 DEG C, keep the temperature charing time be 1~2h.
Step（2）Described in heat temperature raising temperature be 1300~1400 DEG C, reduce temperature be 800~900 DEG C.
Step（3）Described in potassium feldspar and kaolin, silica and aluminium oxide mass ratio be 2:1:1:1, it mixes
It is 10 to close powder and the mass ratio of polyvinyl alcohol and water:1:20.
Step（4）Described in sodium peroxide addition be peach gum quality 10%.
Step（5）Described in ceramic slurry, self-control toughening silicon carbide whisker, cured product and biogas slurry mass ratio be
20:5:1:1, the pressure of tablet press machine is 180~190MPa, a diameter of 20~25mm of ceramic membrane green compact.
Step（6）Described in greenhouse temperature be 40~50 DEG C, relative air humidity be 60~70%.
The beneficial effects of the invention are as follows：
（1）The invention firstly uses the rice husks rich in element silicon as raw material, is carbonized after being rinsed to rice husk so that having in rice husk
Machine matter is at charcoal, and inorganic keel state remains unchanged, and then the rice husk after charing is put into high temperature furnace and is converted, charring rice husk exists
Changed under high temperature, during transformation, charring rice husk still maintains original network-like keel structure, former rice husk surface
Silica convex closure disappear, and form silicon carbide on the original network skeleton of rice husk, finally obtain network-like silicon carbide whisker
Must, using this whisker as toughening material, then take silicate mineral and alumina silica as raw material, using polyvinyl alcohol as
Slurry is prepared in adhesive, coats sodium peroxide followed by peach gum, and by the sodium peroxide and slurry, biogas slurry after cladding
And tabletting is blended in toughening material, finally conserves in the greenhouse, is sintered to get high tenacity porous ceramic film support, wherein originally
The self-control toughening material silicon carbide whisker of invention, since it is with netted keel structure, its incorporation can be as stress biography
The channel passed so that the extraneous stress that ceramic film support is subject to is dispersed into several small parts, to play buffering stress
Effect, increase the toughness of ceramic supporting body；
（2）The present invention is also added into the sodium peroxide and biogas slurry of peach gum cladding in the preparation, and prepares ceramic membrane using it and support
Body green compact put the green body into the greenhouse of high temperature and humidity and conserve, and during maintenance, the microorganism being rich in methane liquid carries out
Fermentation, and microorganism is using peach gum as the nutrient of metabolism, it is constantly uniform during fermentation to discharge carbon dioxide,
Simultaneously with fermentation progress, peach gum gradually by feeding totally, peach gum cladding sodium peroxide therefore be exposed and green compact in
Contact with moisture reaction, generate carbon dioxide collective effect that oxygen and microbial fermentation generate to ceramic film support green compact
It foams, to form uniform hole in green compact, final calcining molding can be obtained high tenacity porous ceramic film
Supporter, ceramic film support porosity produced by the present invention is high, and pore size is uniform, and toughness is strong, before having wide application
Scape.
Specific implementation mode
It weighs rice husk deionized water to rinse 3~5 times, the rice husk after flushing is put into retort, at 400~500 DEG C
Lower heat preservation carbonizes 1~2h, obtains charring rice husk, is 100 in mass ratio by charring rice husk and iron powder:It is packed into vacuum drying oven after 1 mixing
In；It is passed through argon gas into above-mentioned vacuum drying oven with the rate of 50mL/min, is heated to 1300~1400 DEG C under protection of argon gas,
Pyrolytic conversion handles 4~5h, obtains converted product, and stopping is passed through argon gas, and reduces temperature to 800~900 DEG C, keeps the temperature at oxidation
2~3h is managed, then oxidation product hydrofluoric acid is rinsed 3~5 times, obtains self-control toughening silicon carbide whisker；It is 2 in mass ratio:1:
1:1 weighs potassium feldspar and kaolin, silica and aluminium oxide is put into togerther in ball grinder, and 20~30min of milled processed is obtained
It is 10 in mass ratio by mixed-powder and polyvinyl alcohol and water to mixed-powder:1:Ceramic slurry is obtained after 20 mixing, it is standby
With；It weighs peach gum to be put into beaker, beaker is moved into water-bath, increase water-bath pot temperature to 70~80 DEG C, insulated and stirred 20~
30min continuously adds the sodium peroxide of peach gum quality 10% into beaker, continues to be stirred 2~3h, stir until peach gum fusing
It mixes after mixing, natural cooling solidification obtains cured product；By cured product be put into airslide disintegrating mill crush 20~
30min obtains crushed material, is in mass ratio 20:5:1:1 produces spare ceramic slurry, self-control toughening silicon carbide whisker, solidification
After object and biogas slurry mixing in injection stainless steel mould, a diameter of 20 are pressed into the pressure of 180~190MPa with tablet press machine~
The ceramic membrane green compact of 25mm；It is 40~50 DEG C that ceramic membrane green compact, which are put into temperature, the greenhouse that relative air humidity is 60~70%
In, maintenance 2~3 days are stood, the ceramic membrane green compact after maintenance are moved into high-temperature calcination stove, are first heated up with the rate of 5 DEG C/min
To 200 DEG C, 30~35min is kept the temperature, then 1300 DEG C, heat preservation 2~4h of calcining are warming up to the rate program of 3 DEG C/min, calcining knot
Natural cooling discharging is to get high tenacity porous ceramic film support after beam.
It weighs rice husk deionized water to rinse 3 times, the rice husk after flushing is put into retort, charcoal is kept the temperature at 400 DEG C
Change 1h, obtain charring rice husk, is 100 in mass ratio by charring rice husk and iron powder:It is fitted into vacuum drying oven after 1 mixing；With 50mL/
The rate of min is passed through argon gas into above-mentioned vacuum drying oven, is heated to 1300 DEG C under protection of argon gas, and pyrolytic conversion handles 4h,
Obtain converted product, stopping is passed through argon gas, and reduces temperature to 800 DEG C, keeps the temperature oxidation processes 2h, then by oxidation product hydrogen fluorine
Acid rinses 3 times, obtains self-control toughening silicon carbide whisker；It is 2 in mass ratio:1:1:1 weighs potassium feldspar and kaolin, silica
And aluminium oxide is put into togerther in ball grinder, milled processed 20min obtains mixed-powder, by mixed-powder and polyvinyl alcohol with
And water is 10 in mass ratio:1:Ceramic slurry is obtained after 20 mixing, it is spare；It weighs peach gum to be put into beaker, beaker is moved into water
Bath increases water-bath pot temperature to 70 DEG C, and insulated and stirred 20min continuously adds peach gum quality into beaker until peach gum fusing
10% sodium peroxide continues to be stirred 2h, and after being stirred, natural cooling solidification obtains cured product；It will solidification
Product is put into crushing 20min in airslide disintegrating mill and obtains crushed material, is in mass ratio 20:5:1:1 by spare ceramic slurry, from
After toughening silicon carbide whisker, cured product and biogas slurry processed mix in injection stainless steel mould, with tablet press machine with the pressure of 180MPa
It is pressed into the ceramic membrane green compact of a diameter of 20mm；It is 40 DEG C that ceramic membrane green compact, which are put into temperature, the temperature that relative air humidity is 60%
In room, maintenance 2 days are stood, the ceramic membrane green compact after maintenance are moved into high-temperature calcination stove, are first warming up to the rate of 5 DEG C/min
200 DEG C, 30min is kept the temperature, then 1300 DEG C are warming up to the rate program of 3 DEG C/min, 2h is calcined in heat preservation, naturally cold after calcining
But it discharges to get high tenacity porous ceramic film support.
It weighs rice husk deionized water to rinse 4 times, the rice husk after flushing is put into retort, charcoal is kept the temperature at 450 DEG C
Change 1.5h, obtain charring rice husk, is 100 in mass ratio by charring rice husk and iron powder:It is fitted into vacuum drying oven after 1 mixing；With 50mL/
The rate of min is passed through argon gas into above-mentioned vacuum drying oven, is heated to 1350 DEG C under protection of argon gas, pyrolytic conversion processing
4.5h obtains converted product, and stopping is passed through argon gas, and reduces temperature to 850 DEG C, keeps the temperature oxidation processes 2.5h, then oxidation is produced
Object is rinsed 4 times with hydrofluoric acid, obtains self-control toughening silicon carbide whisker；It is 2 in mass ratio:1:1:1 weigh potassium feldspar and kaolin,
Silica and aluminium oxide are put into togerther in ball grinder, and milled processed 25min obtains mixed-powder, by mixed-powder and are gathered
Vinyl alcohol and water are 10 in mass ratio:1:Ceramic slurry is obtained after 20 mixing, it is spare；It weighs peach gum to be put into beaker, will burn
Cup moves into water-bath, increases water-bath pot temperature to 75 DEG C, insulated and stirred 25min is continuously added until peach gum fusing into beaker
The sodium peroxide of peach gum quality 10% continues to be stirred 2.5h, and after being stirred, natural cooling solidification obtains solidification production
Object；Cured product is put into crushing 25min in airslide disintegrating mill and obtains crushed material, is in mass ratio 20:5:1:1 by spare pottery
After porcelain slurry, self-control toughening silicon carbide whisker, cured product and biogas slurry mixing in injection stainless steel mould, with tablet press machine with
The pressure of 185MPa is pressed into the ceramic membrane green compact of a diameter of 22mm；It is 45 DEG C that ceramic membrane green compact, which are put into temperature, and air is opposite
Humidity be 65% greenhouse in, stand maintenance 2 days, by after maintenance ceramic membrane green compact move into high-temperature calcination stove in, first with 5 DEG C/
The rate of min is warming up to 200 DEG C, keeps the temperature 32min, then be warming up to 1300 DEG C, heat preservation calcining 3h with the rate program of 3 DEG C/min,
Natural cooling discharging is to get high tenacity porous ceramic film support after calcining.
It weighs rice husk deionized water to rinse 5 times, the rice husk after flushing is put into retort, charcoal is kept the temperature at 500 DEG C
Change 2h, obtain charring rice husk, is 100 in mass ratio by charring rice husk and iron powder:It is fitted into vacuum drying oven after 1 mixing；With 50mL/
The rate of min is passed through argon gas into above-mentioned vacuum drying oven, is heated to 1400 DEG C under protection of argon gas, and pyrolytic conversion handles 5h,
Obtain converted product, stopping is passed through argon gas, and reduces temperature to 900 DEG C, keeps the temperature oxidation processes 3h, then by oxidation product hydrogen fluorine
Acid rinses 5 times, obtains self-control toughening silicon carbide whisker；It is 2 in mass ratio:1:1:1 weighs potassium feldspar and kaolin, silica
And aluminium oxide is put into togerther in ball grinder, milled processed 30min obtains mixed-powder, by mixed-powder and polyvinyl alcohol with
And water is 10 in mass ratio:1:Ceramic slurry is obtained after 20 mixing, it is spare；It weighs peach gum to be put into beaker, beaker is moved into water
Bath increases water-bath pot temperature to 80 DEG C, and insulated and stirred 30min continuously adds peach gum quality into beaker until peach gum fusing
10% sodium peroxide continues to be stirred 3h, and after being stirred, natural cooling solidification obtains cured product；It will solidification
Product is put into crushing 30min in airslide disintegrating mill and obtains crushed material, is in mass ratio 20:5:1:1 by spare ceramic slurry, from
After toughening silicon carbide whisker, cured product and biogas slurry processed mix in injection stainless steel mould, with tablet press machine with the pressure of 190MPa
It is pressed into the ceramic membrane green compact of a diameter of 25mm；It is 50 DEG C that ceramic membrane green compact, which are put into temperature, the temperature that relative air humidity is 70%
In room, maintenance 3 days are stood, the ceramic membrane green compact after maintenance are moved into high-temperature calcination stove, are first warming up to the rate of 5 DEG C/min
200 DEG C, 35min is kept the temperature, then 1300 DEG C are warming up to the rate program of 3 DEG C/min, 4h is calcined in heat preservation, naturally cold after calcining
But it discharges to get high tenacity porous ceramic film support.
A kind of with the production of Hebei company preparing high tenacity porous ceramic film support as a comparison case using microorganism
To produced by the present invention a kind of using a kind of using micro- in microorganism preparation high tenacity porous ceramic film support and comparative example
Biology prepares high tenacity porous ceramic film support and carries out performance detection, and testing result is as shown in table 1：
1, test method：
Porosity test is detected by 17721 standards of GB T；
Opening size test is detected by GBl967 standards；
Bending strength test is detected by GB/T1964 standards；
Fracture toughness testing is detected by 7732 standards of GB.
1 ceramic film support performance measurement result of table
According to data among the above are produced by the present invention high tenacity porous ceramic film support porosity is prepared using microorganism
Height, material surface is smooth, and even aperture distribution is not easy to plug, and will not cause seriously to pollute, and bending strength reaches 85MPa, and fracture is tough
Degree reaches 8.55MPa/m2, toughness is big, and brittleness is low, and elasticity is big, has broad application prospects.
Claims (7)
1. a kind of method preparing high tenacity porous ceramic film support using microorganism, it is characterised in that specific preparation process
For：
（1）It weighs rice husk deionized water to rinse 3~5 times, the rice husk after flushing is put into retort, heat preservation charing obtains
Charring rice husk is fitted into after mixing charring rice husk and iron powder in vacuum drying oven；
（2）Argon gas is passed through into above-mentioned vacuum drying oven, under protection of argon gas heat temperature raising, pyrolytic conversion handles 4~5h, is converted
Product, stopping is passed through argon gas, and reduces temperature, keeps the temperature 2~3h of oxidation processes, then oxidation product hydrofluoric acid is rinsed 3~5
Time, obtain self-control toughening silicon carbide whisker；
（3）Weigh potassium feldspar and kaolin, silica and aluminium oxide is put into togerther in ball grinder, milled processed 20~
30min obtains mixed-powder, and ceramic slurry is obtained after mixed-powder and polyvinyl alcohol and water are mixed, spare；
（4）It weighs peach gum to be put into beaker, beaker is moved into water-bath, increase water-bath pot temperature to 70~80 DEG C, insulated and stirred
20~30min continuously adds sodium peroxide into beaker, continues to be stirred 2~3h, be stirred end until peach gum fusing
Afterwards, natural cooling cures, and obtains cured product；
（5）Above-mentioned cured product is put into 20~30min of crushing in airslide disintegrating mill and obtains crushed material, by spare ceramic slurry
After material, self-control toughening silicon carbide whisker, above-mentioned cured product and biogas slurry mixing in injection stainless steel mould, it is pressed into tablet press machine
Ceramic membrane green compact；
（6）Above-mentioned ceramic membrane green compact are put into greenhouse, maintenance 2~3 days are stood, the ceramic membrane green compact after maintenance are moved into high temperature
In calcining furnace, 200 DEG C first are warming up to the rate of 5 DEG C/min, keeps the temperature 30~35min, then heat up with the rate program of 3 DEG C/min
To 1300 DEG C, heat preservation 2~4h of calcining, natural cooling discharging is to get high tenacity porous ceramic film support after calcining.
2. a kind of method preparing high tenacity porous ceramic film support using microorganism according to claim 1, special
Sign is：Step（1）Described in heat preservation charing temperature be 400~500 DEG C, keep the temperature charing time be 1~2h.
3. a kind of method preparing high tenacity porous ceramic film support using microorganism according to claim 1, special
Sign is：Step（2）Described in heat temperature raising temperature be 1300~1400 DEG C, reduce temperature be 800~900 DEG C.
4. a kind of method preparing high tenacity porous ceramic film support using microorganism according to claim 1, special
Sign is：Step（3）Described in potassium feldspar and kaolin, silica and aluminium oxide mass ratio be 2:1:1:1, mixing
The mass ratio of powder and polyvinyl alcohol and water is 10:1:20.
5. a kind of method preparing high tenacity porous ceramic film support using microorganism according to claim 1, special
Sign is：Step（4）Described in sodium peroxide addition be peach gum quality 10%.
6. a kind of method preparing high tenacity porous ceramic film support using microorganism according to claim 1, special
Sign is：Step（5）Described in ceramic slurry, self-control toughening silicon carbide whisker, cured product and biogas slurry mass ratio be 20:
5:1:1, the pressure of tablet press machine is 180~190MPa, a diameter of 20~25mm of ceramic membrane green compact.
7. a kind of method preparing high tenacity porous ceramic film support using microorganism according to claim 1, special
Sign is：Step（6）Described in greenhouse temperature be 40~50 DEG C, relative air humidity be 60~70%.
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| CN112774460A (en) * | 2021-01-04 | 2021-05-11 | 江苏新时膜科技有限公司 | Preparation method of high-flux ultrafiltration hollow flat ceramic membrane |
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