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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Abstract
本发明公开了一种低成本高强度氧化铝陶瓷膜支撑体，其特征在于，其原料为两种α‑Al2O3粉末的混合粉末，其中一种α‑Al2O3粉末的中位径为10～30μm，另一种α‑Al2O3粉末的中位径为1～5μm。制备方法为：将混合粉末与溶剂、粘结剂、造孔剂、烧结助剂、消泡剂混合形成浆料；将浆料脱除部分溶剂后形成泥料，泥料通过模具挤压成型形成生坯；生坯经过干燥固化形成煅烧胚品；煅烧胚品在氧气气氛中烧结成为氧化铝陶瓷膜支撑体。本发明所制得的氧化铝陶瓷膜支撑体拥有比传统商品化的氧化铝陶瓷膜支撑体更低的制备成本和更高的抗压强度。The invention discloses a low-cost and high-strength alumina ceramic membrane support, which is characterized in that the raw material is a mixed powder of two kinds of α-Al 2 O 3 powders, and one of the α-Al 2 O 3 powders is a The diameter of the other α-Al 2 O 3 powder is 10-30 μm, and the median diameter of the other α-Al 2 O 3 powder is 1-5 μm. The preparation method is as follows: mixing the mixed powder with a solvent, a binder, a pore-forming agent, a sintering aid and a defoaming agent to form a slurry; removing part of the solvent from the slurry to form a mud, and the mud is formed by extrusion molding through a die green body; the green body is dried and solidified to form a calcined embryo; the calcined embryo is sintered in an oxygen atmosphere to become an alumina ceramic membrane support. The alumina ceramic membrane support body prepared by the invention has lower preparation cost and higher compressive strength than the traditional commercial alumina ceramic membrane support body.
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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