CN109400132A - A kind of low-cost high-strength aluminium oxide ceramics film support and preparation method thereof - Google Patents
A kind of low-cost high-strength aluminium oxide ceramics film support and preparation method thereof Download PDFInfo
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- CN109400132A CN109400132A CN201811275869.1A CN201811275869A CN109400132A CN 109400132 A CN109400132 A CN 109400132A CN 201811275869 A CN201811275869 A CN 201811275869A CN 109400132 A CN109400132 A CN 109400132A
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- aluminium oxide
- oxide ceramics
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- ceramics film
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000000919 ceramic Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 239000011812 mixed powder Substances 0.000 claims abstract description 13
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 238000007711 solidification Methods 0.000 claims abstract description 7
- 230000008023 solidification Effects 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 210000001161 mammalian embryo Anatomy 0.000 claims abstract description 6
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 5
- 239000011230 binding agent Substances 0.000 claims abstract description 5
- 239000011148 porous material Substances 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000001125 extrusion Methods 0.000 claims abstract description 3
- 239000012046 mixed solvent Substances 0.000 claims abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- -1 sintering aid Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 13
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 13
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 7
- 239000004115 Sodium Silicate Substances 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 6
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 5
- 239000005751 Copper oxide Substances 0.000 claims description 4
- 229910000431 copper oxide Inorganic materials 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 3
- 229920002472 Starch Polymers 0.000 claims description 3
- 239000013530 defoamer Substances 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 235000019698 starch Nutrition 0.000 claims description 3
- 239000008107 starch Substances 0.000 claims description 3
- 235000011194 food seasoning agent Nutrition 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 230000006835 compression Effects 0.000 abstract description 14
- 238000007906 compression Methods 0.000 abstract description 14
- 230000008859 change Effects 0.000 abstract description 2
- 239000012528 membrane Substances 0.000 description 12
- 230000004907 flux Effects 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 5
- 238000000926 separation method Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a kind of low-cost high-strength aluminium oxide ceramics film supports, which is characterized in that its raw material is two kinds of α-Al2O3The mixed-powder of powder, one of α-Al2O3The meso-position radius of powder is 10~30 μm, another α-Al2O3The meso-position radius of powder is 1~5 μm.The preparation method comprises the following steps: mixed-powder and solvent, binder, pore creating material, sintering aid, defoaming agent are mixed to form slurry；Pug is formed after slurry is removed partial solvent, pug forms green compact by mold extrusion forming；Green compact form calcining embryo product by dry solidification；Calcining embryo product are sintered into aluminium oxide ceramics film support in oxygen atmosphere.Aluminium oxide ceramics film support obtained by the present invention possesses preparation cost more lower than the aluminium oxide ceramics film support of traditional commodities change and higher compression strength.
Description
Technical field
The present invention relates to a kind of ceramic film supports and preparation method thereof, and in particular to a kind of low-cost high-strength oxidation
Aluminium ceramic film support and preparation method thereof.
Background technique
Membrane separation technique is the isolation technics of an economical and efficient.Since it has separation, concentration, purifying and purification
Function, but have both efficiently, energy-saving and environmental protection, using easy, the low series of advantages of energy consumption, be widely used in food, medicine,
The fields such as biology, environmental protection, chemical industry, the energy, water process, it has also become one of most important means in current separation science.Wherein,
Ceramic membrane technology starts from atom bomb plan in World War II, with the development of material technology and its universal, the ceramics of intrinsic advantage
The technology of preparing of film is becoming the focus and emphasis of various countries' development in science and technology.Ceramic membrane be one kind with inorganic material through special work
Skill preparation and formed anisotropic membrane, compared to organic film have better chemical stability, acid-fast alkali-proof, organic solvent-resistant,
Numerous advantages such as resistance to bacterium, high temperature resistant, high mechanical strength, separation process simple, simple and convenient operation and maintenance, long service life, obtain
It is extensive to pay attention to and apply.
In existing technology, the aluminium oxide ceramics film support of commercialization usually require hot conditions (1700 DEG C with
On) under for a long time (at a sintering temperature soaking time usually >=2h) be sintered, this considerably increases alumina ceramic membrane branch
The preparation cost of support body realizes the cost effective production of ceramic membrane, in conjunction with the membrane material design and system of building application-orientation
Preparation Method solves the bottleneck problem that ceramic membrane promotes and applies, this is following developing direction.Simultaneously as intensity is insufficient,
Supporter needs thicker thickness, therefore the membrane area in its channel is smaller, causes the integrated level of ceramic membrane filter equipment low,
Equipment manufacturing cost is expensive, and operating cost is high, limits ceramic membrane in the application in the fields such as water process, water-oil separating.
Summary of the invention
Problem to be solved by this invention is: providing a kind of with high-intensitive, high-purity water flux, low preparation cost
Aluminium oxide ceramics film support and its manufacturing method.
To solve the above-mentioned problems, technical scheme is as follows:
A kind of low-cost high-strength aluminium oxide ceramics film support, which is characterized in that its raw material is two kinds of α-Al2O3Powder
Mixed-powder, one of α-Al2O3The meso-position radius of powder is 10~30 μm, another α-Al2O3The meso-position radius of powder is 1
~5 μm.
Preferably, two kinds of α-Al2O3The mass ratio of powder is 1:1.
The present invention also provides a kind of preparation methods of above-mentioned low-cost high-strength aluminium oxide ceramics film support, special
Sign is, comprising the following steps:
Step 1): mixed-powder and solvent, binder, pore creating material, sintering aid, defoaming agent are mixed to form slurry；
Step 2): pug is formed after slurry is removed partial solvent, pug forms green compact by mold extrusion forming；
Step 3): green compact form calcining embryo product by dry solidification；
Step 4): calcining embryo product are sintered into aluminium oxide ceramics film support in oxygen atmosphere.
Preferably, in the step 1) solvent dosage be mixed-powder weight 20%-30%；Solvent uses water.
Preferably, the binder in the step 1) uses the polyvinyl alcohol of the degree of polymerization 1750 ± 50, and pore creating material uses can
Soluble starch, sintering aid use one or more of titanium dioxide, magnesia, manganese dioxide, copper oxide and sodium metasilicate,
Total dosage of three is the 10-15% of mixed-powder weight.
It is highly preferred that when the sintering aid is titanium dioxide, magnesia, manganese dioxide, copper oxide or sodium metasilicate,
Its corresponding dosage respectively is 2%, 0.5%, 1.5%, 1.5%, the 4% of mixed powder weight.It is preferred that being burnt using quaternary
Tie auxiliary agent (0.5%MgO+2%TiO2+ 1.5%MnO2+ 1.5%CuO) reduce sintering temperature, increase compression strength.Wherein
MgO can form liquid phase at a lower temperature, and liquid phase flows between particle, infiltrate and surround powder granule, produce powder granule
Life competitively connects, and mechanism of mass transfer is made to be changed into liquid phase diffusion by solid-state diffusion, forms glass phase to reduce sintering temperature.
TiO2、MnO2, CuO utilize particle radii and Al3+Difference activated Al in addition itself being transition-metal ions2O3The crystalline substance of crystal
Lattice generate intermediate solid solution to reduce sintering temperature and improve the compression strength of supporter.Prepared ceramic film support
Diameter is in 7.8-8.2cm, and thickness is in 5-7mm, and pure water flux is in 8000-9000Lm-2·h-1·bar-1, porosity exists
30%-38%, compression strength is in 20-50MPa.
Preferably, the defoaming agent in the step 1) is organic silicon defoamer, and dosage is the 1%- of mixed-powder weight
5%, preferably 5%.
Preferably, the dry solidification mode in the step 3) uses natural seasoning, and it is many to be dried at room temperature for solidification
In 1 day.
Preferably, the temperature being sintered in the step 4) is 1450 DEG C, soaking time 0.5-2h.It is prepared by the present invention
Aluminium oxide ceramics film support uses the α-Al of specified particle size gradation2O3Arrange in pairs or groups, in 1450 DEG C of low temperature the short time (≤
It 2h) is sintered, comprehensively considers the overall performance of sintering cost and support, the preferably sintered heat insulating time is 1h, and ceramic membrane support is made
Body.
Aluminium oxide ceramics film support obtained by the present invention possesses the aluminium oxide ceramics film support than traditional commodities change
Lower preparation cost and higher compression strength.
Specific embodiment
In order to make the present invention more obvious and understandable, it hereby with preferred embodiment, and is described in detail below.
Embodiment 1
A kind of preparation method of low-cost high-strength aluminium oxide ceramics film support:
1) α-Al for being 10 μm by meso-position radius2O3Powder 100g, the α-Al that meso-position radius is 3 μm2O3Powder 100g, sodium metasilicate
8g takes suitable quantity of water to dissolve, and forms sodium silicate solution；
2) soluble starch 12g, dissolution forms colloidal sol in 80 DEG C of water；
3) PVA (degree of polymerization 1750 ± 50) 1.2g dissolves complete in 85 DEG C of water；
4) by above-mentioned each substance and MgO 1g, TiO28g mixing after, the water of 45mL is added, with homogeneous blender with
The speed of 1800r/min stirs 30min, is uniformly mixed slurry, then 10g organic silicon defoamer is added in the slurry and is surpassing
30min is placed in sound+Suction filtration device removes bubble；
5) slurry after deaeration is dehydrated in 100 DEG C of baking ovens 1h, forms pug, pug is squeezed with every part of 100g
It is squeezed in formula circular die and forms green compact, dried 1 day at room temperature；
6) it in air atmosphere, is put in Muffle furnace and is increased to 200 DEG C from 50 DEG C with the rate of 3 DEG C/min, and keep the temperature
30min；It is increased to 1000 DEG C from 200 DEG C with the rate of 5 DEG C/min, keeps the temperature 30min；It is risen with the rate of 3 DEG C/min from 1000 DEG C
Up to 1450 DEG C, and keep the temperature 2h.
Obtained aluminium oxide ceramics film support diameter is 8cm, and with a thickness of 4mm, pure water flux is 8482 Lm-2·h-1·bar-1, porosity 31.3%, compression strength 27.3MPa.
Embodiment 2
The present embodiment difference from example 1 is that, TiO in step 4)2It is replaced with CuO 3g.
Obtained aluminium oxide ceramics film support diameter is 7.8cm, and with a thickness of 5mm, pure water flux is 8342 Lm-2·
h-1·bar-1, porosity 35.2%, compression strength 20.1MPa.
Embodiment 3
The present embodiment difference from example 1 is that, TiO in step 4)2Use MnO23g is replaced.
Obtained aluminium oxide ceramics film support diameter is 8.3cm, and with a thickness of 4mm, pure water flux is 8791 Lm-2·
h-1·bar-1, porosity 30.0%, compression strength 15.3MPa.
Embodiment 4
The present embodiment difference from example 1 is that, sintering aid increases CuO 3g in step 4).
Obtained aluminium oxide ceramics film support diameter is 8.1cm, and with a thickness of 5mm, pure water flux is 8123 Lm-2·
h-1·bar-1, porosity 33.4%, compression strength 35.6MPa.
Embodiment 5
The present embodiment difference from example 1 is that, sintering aid increases MnO in step 4)2 3g。
Obtained aluminium oxide ceramics film support diameter is 7.9cm, and with a thickness of 4mm, pure water flux is 8319 Lm-2·
h-1·bar-1, porosity 38.3%, compression strength 30.1MPa.
Embodiment 6
The present embodiment difference from example 1 is that, sintering aid increases CuO 3g, MnO in step 4)2
3g。
Obtained aluminium oxide ceramics film support diameter is 8.0cm, and with a thickness of 5mm, pure water flux is 8521 Lm-2·
h-1·bar-1, porosity 35.8%, compression strength 45.9MPa.
Embodiment 7
The present embodiment and embodiment 6 the difference is that, keep the temperature 0.5h after 1450 DEG C are risen in the step 6).
Obtained aluminium oxide ceramics film support diameter is 8.0cm, and with a thickness of 5mm, pure water flux is 9146 Lm-2·
h-1·bar-1, porosity 38.5%, compression strength 25.2MPa.
Embodiment 8
The present embodiment and embodiment 6 the difference is that, keep the temperature 1h after 1450 DEG C are risen in the step 6).
Obtained aluminium oxide ceramics film support diameter is 8.3cm, and with a thickness of 4mm, pure water flux is 8945 Lm-2·
h-1·bar-1, porosity 36.9%, compression strength 38.4MPa.
Embodiment 9
The present embodiment and embodiment 6 the difference is that, keep the temperature 1.5h after 1450 DEG C are risen in the step 6).
Obtained aluminium oxide ceramics film support diameter is 7.8cm, and with a thickness of 5mm, pure water flux is 8672 Lm-2·
h-1·bar-1, porosity 37.1%, compression strength 42.3MPa.
Claims (9)
1. a kind of low-cost high-strength aluminium oxide ceramics film support, which is characterized in that its raw material is two kinds of α-Al2O3Powder
Mixed-powder, one of α-Al2O3The meso-position radius of powder is 10~30 μm, another α-Al2O3The meso-position radius of powder is 1~5
μm。
2. low-cost high-strength aluminium oxide ceramics film support as described in claim 1, which is characterized in that two kinds of α-
Al2O3The mass ratio of powder is 1:1.
3. a kind of preparation method of low-cost high-strength aluminium oxide ceramics film support of any of claims 1 or 2, feature exist
In, comprising the following steps:
Step 1): mixed-powder and solvent, binder, pore creating material, sintering aid, defoaming agent are mixed to form slurry；
Step 2): pug is formed after slurry is removed partial solvent, pug forms green compact by mold extrusion forming；
Step 3): green compact form calcining embryo product by dry solidification；
Step 4): calcining embryo product are sintered into aluminium oxide ceramics film support in oxygen atmosphere.
4. the preparation method of low-cost high-strength aluminium oxide ceramics film support as claimed in claim 3, which is characterized in that institute
The dosage for stating solvent in step 1) is the 20%-30% of mixed-powder weight；Solvent uses water.
5. the preparation method of low-cost high-strength aluminium oxide ceramics film support as claimed in claim 3, which is characterized in that institute
The polyvinyl alcohol that the binder in step 1) uses the degree of polymerization 1750 ± 50 is stated, pore creating material uses soluble starch, sintering aid
Using one or more of titanium dioxide, magnesia, manganese dioxide, copper oxide and sodium metasilicate, total dosage of three is mixing
The 10-15% of powder weight.
6. the preparation method of low-cost high-strength aluminium oxide ceramics film support as claimed in claim 5, which is characterized in that when
When the sintering aid is titanium dioxide, magnesia, manganese dioxide, copper oxide or sodium metasilicate, corresponding dosage is successively distinguished
It is 2%, 0.5%, 1.5%, 1.5%, the 4% of mixed powder weight.
7. the preparation method of low-cost high-strength aluminium oxide ceramics film support as claimed in claim 3, which is characterized in that institute
Stating the defoaming agent in step 1) is organic silicon defoamer, and dosage is the 1%-5% of mixed-powder weight.
8. the preparation method of low-cost high-strength aluminium oxide ceramics film support as claimed in claim 3, which is characterized in that institute
The dry solidification mode in step 3) is stated using natural seasoning, is dried at room temperature for solidification no less than 1 day.
9. the preparation method of low-cost high-strength aluminium oxide ceramics film support as claimed in claim 3, which is characterized in that institute
Stating the temperature being sintered in step 4) is 1450 DEG C, soaking time 0.5-2h.
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| CN111545078A (en) * | 2020-05-15 | 2020-08-18 | 洛阳中超新材料股份有限公司 | Flat ceramic membrane and preparation method thereof |
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| CN114133270A (en) * | 2021-12-28 | 2022-03-04 | 攀枝花学院 | Hollow flat ceramic filter membrane and preparation method thereof |
| CN114452834B (en) * | 2022-01-18 | 2023-11-03 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane |
| CN114452834A (en) * | 2022-01-18 | 2022-05-10 | 重庆兀盾纳米科技有限公司 | Disc type ceramic membrane |
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