CN106007779B - The preparation method of high purity aluminium oxide flat ceramic film support - Google Patents
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- 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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Abstract
The present invention provides a kind of preparation method of high purity aluminium oxide flat ceramic film support, includes the following steps：Step 1: zirconium nitrate is put into deionized water heating stirring；Step 2: by aluminium oxide a, aluminium oxide b, lanthana；The powder of yttrium oxide, which is proportionally added into kneader, to be mixed；Step 3: the mixture of step 1 and step 2 is mixed；Step 4: being sufficiently mixed after dextrin, PVA, glycerine, tung oil are weighed in proportion, it is added in the material in step 3 and mixes, obtain pug；Step 5: pug is moved into pugging in pug mill, it is then placed in extruder, by idiosome naturally dry after extrusion；It is dried Step 6: idiosome is put into baking oven, idiosome is put into kiln and is sintered.The alumina content for the flat ceramic film support that the present invention prepares is more than 99%, while greatly improving the corrosion-resistant service life emphasized with ceramic membrane of supporter, also ensures that ceramic membrane can be in the use steady in a long-term under alkali system.
Description
Technical field
The present invention relates to a kind of preparation methods of high purity aluminium oxide flat ceramic film support, belong to ceramic field.
Background technology
Membrane separation technique originates from early 20th century, is widely used in food, medicine, biology, ring after the 1960s
The various fields such as guarantor, chemical industry, metallurgy, the energy, oil, water process have become one of most important separation means.From shape
On, film is broadly divided into：Plate membrane, tubular membrane, hollow-fibre membrane, rolled film etc..
At present mostly based on organic material, major part is Kynoar (PVDF), gathers the plate membrane of water treatment field
Vinyl chloride (PVC) etc., but the inoxidizability of organic film and hydrophily difference cause low separation efficiency, service life shorter, and limiting it makes
With range, in particular for complicated component, there is the industrial wastewater of stronger acids basicity.Ceramic membrane has incomparable excellent of organic film
Point, such as：High temperature resistant, good hydrophilic property, strong alkali-acid resistance, organic solvent-resistant.
But the ceramic membrane produced both at home and abroad is mostly tubular type multichannel, and the short slab of tubular ceramic membrane is：Loading density is low, is not easy
Regeneration, transmembrane pressure lead to greatly high energy consumption.These disadvantages limit a wide range of use of the tubular ceramic membrane in water treatment field.
Ceramic membrane combines the advantages of tablet organic film and tubular ceramic membrane just, convenient in Treatment of Industrial Water, object
The popularization and application in the fields such as material separation.However, existing flat ceramic film support alumina content is not high, lead to not strong
It is used steadily in the long term under the system of sour highly basic, moreover, existing ceramic membrane supporting body surface finish is not high, leads to film
Overweight coating influences service efficiency etc..
Invention content
The purpose of the present invention is to provide a kind of preparation methods of high purity aluminium oxide flat ceramic film support, in solution
State problem.
Present invention employs following technical solutions：
A kind of preparation method of high purity aluminium oxide flat ceramic film support, which is characterized in that include the following steps：
Step 1: 16~10 parts of zirconium nitrates to be put into 660~540 parts of deionized water heating stirring；
Step 2: by aluminium oxide a, aluminium oxide b, lanthana；2750~2250 parts in proportion of the powder of yttrium oxide:451 parts
~369 parts:11~9 parts:It is mixed in 4.95~4.05 parts of addition kneaders, the D50 of wherein aluminium oxide a is：20 μm -35 μm, oxygen
The D50 for changing aluminium b is：2.5μm-5μm；
Step 3: in the mixture that the liquid obtained in step 1 addition step 2 is obtained, it is sufficiently mixed；
Step 4: by 209~171 parts in proportion of dextrin, PVA, glycerine, tung oil organic additive:214.5~175.5 parts:
77~63 parts:49.5~40.5 parts weigh after, be sufficiently mixed, by the organic additive mixed slowly, be homogeneously added into step
In material in rapid three, kneader should be under admixture during addition, mixes 15 minutes, obtains pug；
Step 5: kneaded pug is moved into pugging in pug mill, it is then placed in extruder and is squeezed out, after extrusion
Idiosome naturally dry；
It is dried Step 6: idiosome after natural drying is put into baking oven, after drying, idiosome is put into kiln after testing
Middle sintering gradually heats up, and sintering temperature is 1500-1700 DEG C.
Further, the preparation method of high purity aluminium oxide flat ceramic film support of the invention can also have such
Feature：Wherein, in step 1,90 DEG C of whens, are slowly added to 1 part of oxalic acid, and constant temperature stops heating and stirring is maintained to be cooled to room after 36 hours
Temperature.
Further, the preparation method of high purity aluminium oxide flat ceramic film support of the invention can also have such
Feature：Incorporation time in step 2 was at 30 minutes or more.
Further, the preparation method of high purity aluminium oxide flat ceramic film support of the invention can also have such
Feature：In step 5, first it is kneaded 5 times in air when pugging, then pugging 5 times under the vacuum degree of 0.10MPa.
Further, the preparation method of high purity aluminium oxide flat ceramic film support of the invention can also have such
Feature：In step 5, the time of naturally dry is at least 3 days.
Further, the preparation method of high purity aluminium oxide flat ceramic film support of the invention can also have such
Feature：In step 6, heating rate is 2-6 DEG C/min.
Further, the preparation method of high purity aluminium oxide flat ceramic film support of the invention can also have such
Feature：In step 6,2-4 hours are kept the temperature after reaching sintering temperature.
Further, the preparation method of high purity aluminium oxide flat ceramic film support of the invention can also have such
Feature：Wherein, the D50 of lanthana is less than 4 microns.
Further, the preparation method of high purity aluminium oxide flat ceramic film support of the invention can also have such
Feature：Wherein, the D50 of yttrium oxide is less than 4 microns.
Further, the preparation method of high purity aluminium oxide flat ceramic film support of the invention can also have such
Feature：In step 5, idiosome after extrusion is placed on smooth plank by when naturally dry to be dried.
Advantageous effect of the invention
The alumina content for the flat ceramic film support prepared using the present invention is more than 99%, and uses other methods
It prepares or ceramic film support alumina content in the market is not more than 97%, greatly improve the corrosion-resistant of supporter and emphasize and make pottery
While the service life of porcelain film, also ensure that ceramic membrane can be in the use steady in a long-term under alkali system.
The porosity for the flat ceramic film support that the present invention prepares is 30-50%, and average pore size is 5-7 μm, pure water
Flux is 10-20m3.m-2.h-1.bar-1, compression strength is more than 80MPa.
The surface smoothness for the flat ceramic film support that the present invention prepares is high, can reduce the coating thickness of separating layer,
The osmotic resistance of anisotropic membrane is greatly reduced.
The preparation method of the high purity aluminium oxide flat ceramic film support of the present invention, due to adding the colloid of zirconium nitrate,
Therefore the effect of ceramic post sintering is more preferable, and the range in the aperture inside ceramics is narrower, and the size in aperture is evenly in other words.
In addition, as a result of the alumina powder of two kinds of particle sizes, therefore bigger is formd in sintering process
Hole so that after ceramic membrane is made using the supporter of the present invention, filter efficiency increases substantially.
Description of the drawings
Fig. 1 is the overall structure signal of high purity aluminium oxide flat ceramic film support made from method using the present invention
Figure；
Fig. 2 is the scanning electron microscope (SEM) photograph of high purity aluminium oxide flat ceramic film support made from method using the present invention.
Specific implementation mode
Illustrate the specific implementation mode of the present invention below in conjunction with attached drawing.
<Embodiment one>
1) 160g zirconium nitrates are put into 6.6L deionized water heating stirrings, 90 DEG C of whens are slowly added to 10g oxalic acid, and constant temperature 36 is small
When after stop heating maintain stirring be cooled to room temperature, it is spare；
2) it is by aluminium oxide a, D50：20μm-35μm；Aluminium oxide b, D50 are：2μm-5μm；Lanthana；Yttrium oxide etc.
Inorganic powder 27500g in proportion:4510g:110g:It is mixed 1 hour 49.5g being added in kneader；
3) mixed liquor that step 1) obtains is added in the mixture obtained in step 2), is sufficiently mixed 30 minutes；
4) by the organic additives such as dextrin, PVA, glycerine, tung oil 2090g in proportion:2145g:770g:495g precises
Afterwards, it is sufficiently mixed, in the state that inorganic powder mixes in kneader, slowly, is homogeneously added into the organic addition mixed
Agent mixes 30 minutes；
5) kneaded pug is moved into vacuum deairing machine, is first kneaded 5 times under normobaric air conditions, then
Pugging 5 times, are then placed in extruder under the vacuum degree of 0.10MPa, by dedicated extrusion die, extrusion pressure 3.0MPa.
It controls temperature and is no more than 40 DEG C.Idiosome after extrusion is placed on smooth plank, is tilted 20 degree and is put, naturally dry.Use tablet
The mold of ceramic membrane is squeezed out.
6) after 4 days dry, idiosome is put into baking oven and is dried, oven temperature is 110 DEG C, total drying time
It is 24 hours.After drying, idiosome is put into shuttle kiln is sintered after testing, heating rate is 3 DEG C/min, and sintering temperature is
1700 DEG C, 3 hours are kept the temperature, obtains high purity aluminium oxide flat ceramic film support product, the structure of this product is as shown in Figure 1, production
Product generally tabular, Fig. 1 present the cross section structure of tablet, and the size of each part is as follows：A=145mm；B=6.00mm；C=
3.50mm；D=3.24m；E=1.25mm.After testing, the aluminium oxide of flat ceramic film support obtained contains in present embodiment
Amount is 99.3%.
<Embodiment two>
1) 130g zirconium nitrates are put into 6L deionized water heating stirrings, 90 DEG C of whens are slowly added to 10g oxalic acid, constant temperature 36 hours
Stopping heating afterwards maintains stirring to be cooled to room temperature, spare；
2) it is by aluminium oxide a, D50：20μm-35μm；Aluminium oxide b, D50 are：2 μm -5 μm, lanthana, yttrium oxide etc.
Inorganic powder 25000g in proportion:4100g:100g:45g is added in kneader and mixes 1 hour；
3) mixed liquor that step 1) obtains is added in the mixture obtained in step 2), is sufficiently mixed 1 hour；
4) by the organic additives such as dextrin, PVA, glycerine, tung oil 1900g in proportion:1950g:700g:450g precises
Afterwards, it is sufficiently mixed, in the state that inorganic powder mixes in kneader, slowly, is homogeneously added into the organic addition mixed
Agent mixes 30 minutes；
5) kneaded pug is moved into vacuum deairing machine, is first kneaded 5 times under normobaric air conditions, then
Pugging 5 times, are then placed in extruder under the vacuum degree of 0.10MPa, by dedicated extrusion die, extrusion pressure 3.5MPa.
It controls temperature and is no more than 40 DEG C.Idiosome after extrusion is placed on smooth plank, is tilted 30 degree and is put, naturally dry.Use tablet
The mold of ceramic membrane is squeezed out.
6) after 4 days dry, idiosome is put into baking oven and is dried, oven temperature is 120 DEG C, total drying time
It is 24 hours.After drying, idiosome is put into shuttle kiln is sintered after testing, heating rate is 3 DEG C/min, and sintering temperature is
1650 DEG C, 3 hours are kept the temperature, high purity aluminium oxide flat ceramic film support product is obtained.Use the height obtained by present embodiment
The scanning electron microscope (SEM) photograph of pure alumina flat ceramic film support, as shown in Figure 2, it is seen that its hole is uniform, and structure is neat, surface light
Cleanliness is high.The macrostructure for the product that present embodiment obtains is identical as in embodiment one, and details are not described herein again.After testing,
The alumina content of flat ceramic film support obtained is 99.8% in present embodiment.
<Embodiment three>
1) 100g zirconium nitrates are put into 5.4L deionized water heating stirrings, 90 DEG C of whens are slowly added to 10g oxalic acid, and constant temperature 36 is small
When after stop heating maintain stirring be cooled to room temperature, it is spare；
2) it is by aluminium oxide a, D50：20μm-35μm；Aluminium oxide b, D50 are：2μm-5μm；Lanthana；Yttrium oxide this
Several inorganic powders 22500g in proportion:3690g:90g:40.5g is added in kneader and mixes 1 hour；
3) mixed liquor that step 1) obtains is added in the mixture obtained in step 2), is sufficiently mixed 30 minutes；
4) by the organic additives such as dextrin, PVA, glycerine, tung oil 1710g in proportion:1755g:630g:405g precises
Afterwards, it is sufficiently mixed, in the state that inorganic powder mixes in kneader, slowly, is homogeneously added into the organic addition mixed
Agent mixes 30 minutes；
5) kneaded pug is moved into vacuum deairing machine, is first kneaded 5 times under normobaric air conditions, then
Pugging 5 times, are then placed in extruder under the vacuum degree of 0.10MPa, by dedicated extrusion die, extrusion pressure 4.0MPa.
It controls temperature and is no more than 40 DEG C.Idiosome after extrusion is placed on smooth plank, is tilted 40 degree and is put, naturally dry.Use tablet
The mold of ceramic membrane is squeezed out.
6) after 3 days dry, idiosome is put into baking oven and is dried, oven temperature is 150 DEG C, total drying time
It is 24 hours.After drying, idiosome is put into shuttle kiln is sintered after testing, heating rate is 3 DEG C/min, and sintering temperature is
1500 DEG C, 3 hours are kept the temperature, high purity aluminium oxide flat ceramic film support product is obtained.The product that present embodiment obtains it is macro
Sight structure is identical as in embodiment one, and details are not described herein again.After testing, ceramic membrane support obtained in present embodiment
The alumina content of body is 99.4%.
Claims (9)
1. a kind of preparation method of high purity aluminium oxide flat ceramic film support, which is characterized in that include the following steps：
Step 1: 16~10 parts of zirconium nitrates to be put into 660~540 parts of deionized water heating stirring, 90 DEG C of whens, are slowly added to 1 part
Oxalic acid, constant temperature stop heating and stirring are maintained to be cooled to room temperature after 36 hours；
Step 2: by aluminium oxide a, aluminium oxide b, lanthana；2750~2250 parts in proportion of the powder of yttrium oxide:451 parts~369
Part:11~9 parts:It is mixed in 4.95~4.05 parts of addition kneaders, the D50 of wherein aluminium oxide a is：20 μm -35 μm, aluminium oxide b
D50 be：2.5μm-5μm；
Step 3: in the mixture that the liquid obtained in step 1 addition step 2 is obtained, it is sufficiently mixed；
Step 4: by 209~171 parts in proportion of dextrin, PVA, glycerine, tung oil organic additive:214.5~175.5 parts:77~
63 parts:49.5~40.5 parts weigh after, be sufficiently mixed, by the organic additive mixed slowly, be homogeneously added into step 3
In material in, kneader should be under admixture during addition, mix 15 minutes, obtain pug；
Step 5: kneaded pug is moved into pugging in pug mill, it is then placed in extruder and is squeezed out, by embryo after extrusion
Body naturally dry；
It is dried Step 6: idiosome after natural drying is put into baking oven, after drying, idiosome is put into kiln burns after testing
Knot gradually heats up, and sintering temperature is 1500-1700 DEG C.
2. the preparation method of high purity aluminium oxide flat ceramic film support as described in claim 1, it is characterised in that：
Incorporation time in step 2 was at 30 minutes or more.
3. the preparation method of high purity aluminium oxide flat ceramic film support as described in claim 1, it is characterised in that：
In step 5, first it is kneaded 5 times in air when pugging, then pugging 5 times under the vacuum degree of 0.10MPa.
4. the preparation method of high purity aluminium oxide flat ceramic film support as described in claim 1, it is characterised in that：
In step 5, the time of naturally dry is at least 3 days.
5. the preparation method of high purity aluminium oxide flat ceramic film support as described in claim 1, it is characterised in that：
In step 6, heating rate is 2-6 DEG C/min.
6. the preparation method of high purity aluminium oxide flat ceramic film support as described in claim 1, it is characterised in that：
In step 6,2-4 hours are kept the temperature after reaching sintering temperature.
7. the preparation method of high purity aluminium oxide flat ceramic film support as described in claim 1, it is characterised in that：
Wherein, the D50 of lanthana is less than 4 microns.
8. the preparation method of high purity aluminium oxide flat ceramic film support as described in claim 1, it is characterised in that：
Wherein, the D50 of yttrium oxide is less than 4 microns.
9. the preparation method of high purity aluminium oxide flat ceramic film support as described in claim 1, it is characterised in that：
In step 5, idiosome after extrusion is placed on smooth plank by when naturally dry to be dried.
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| CN108435000B (en) * | 2017-02-16 | 2023-12-08 | 上海硅苑膜科技有限公司 | Automatic film coating device for flat ceramic film and preparation method of flat ceramic film |
| CN109574635A (en) * | 2018-12-19 | 2019-04-05 | 杭州大和江东新材料科技有限公司 | A kind of preparation method of semiconductor grade extrusion molding high-purity alumina ceramic product |
| CN115231902A (en) * | 2022-07-10 | 2022-10-25 | 上海熊猫机械(集团)有限公司 | W-type alumina-supported silicon carbide ceramic membrane and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101139206A (en) * | 2007-08-13 | 2008-03-12 | 南京九思高科技有限公司 | Method for preparing low-temperature burnt porous ceramics support |
| CN103755328A (en) * | 2014-02-07 | 2014-04-30 | 刘旭红 | Preparation method of tubular ceramic membrane support body |
| CN105565785A (en) * | 2015-12-25 | 2016-05-11 | 山东硅元新型材料有限责任公司 | Preparation method of ceramic membrane support body |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101139206A (en) * | 2007-08-13 | 2008-03-12 | 南京九思高科技有限公司 | Method for preparing low-temperature burnt porous ceramics support |
| CN103755328A (en) * | 2014-02-07 | 2014-04-30 | 刘旭红 | Preparation method of tubular ceramic membrane support body |
| CN105565785A (en) * | 2015-12-25 | 2016-05-11 | 山东硅元新型材料有限责任公司 | Preparation method of ceramic membrane support body |
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