CN109534819A - Filter plate ceramic membrane and preparation method thereof - Google Patents
Filter plate ceramic membrane and preparation method thereof Download PDFInfo
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- CN109534819A CN109534819A CN201710865140.9A CN201710865140A CN109534819A CN 109534819 A CN109534819 A CN 109534819A CN 201710865140 A CN201710865140 A CN 201710865140A CN 109534819 A CN109534819 A CN 109534819A
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Abstract
The invention discloses a kind of filter plate ceramic membranes, it forms the component including following parts by weight: 60~80 parts of silicon carbide, 5~10 parts of silicon nitride, 5~8 parts of aluminium oxide, 3~6 parts of magnesia, 1~3 part of neodymia, 0.1~1 part of polyacrylic acid, 10~20 parts of styrene-acrylate emulsion, 0.1~0.5 part of polyvinyl alcohol.Above-mentioned ceramic membrane is prepared using the tape casting and cement-dipping method.The temperature in each stage when by each component ratio and sintering, and sintering temperature is reduced by the way that aluminium oxide, magnesia, neodymia etc. is added, improve the bond strength of silicon carbide and silicon nitride, to obtain high-intensitive supporter and film layer, the porosity of the ceramic membrane can achieve 40%, intensity reaches 20Mpa, and filter hole pore size control is in 50~80nm.
Description
Technical field
The present invention relates to a kind of filter mediums, more particularly, to a kind of flat ceramic membrane filter media, while being related to its system
Preparation Method.
Background technique
Ceramic membrane is one of inoranic membrane, belongs to the solid membrane material in membrane separation technique, mainly with different size
The inorganic ceramic materials such as aluminium oxide, zirconium oxide, titanium oxide and silica are fired as supporter through surface coating, high temperature.
Separation ceramic membrane usually has three-decker: supporter (also known as carrier layer), transition zone (also known as middle layer), film layer are (also known as
Separating layer), wherein the effect of supporting layer is to increase the mechanical strength of film；The aperture of the aperture ratio supporting layer of middle layer is small, makees
With being to prevent infiltration of the particle to porous support layer in film layer preparation process；Film layer has separation function.The aperture point of entire film
Cloth is gradually reduced by supporting layer to film layer, forms asymmetric structure distribution.According to the difference of supporter, the configuration of ceramic membrane can
It is divided into plate, tubular type, three kinds of multichannel.Chinese patent application CN201310325539.X discloses a kind of earthenware slab film support
Body obtains asymmetric plate membrane by preparing half of film using the tape casting, and Chinese patent application CN201710170386.4 is disclosed
A kind of Water warfare earthenware slab film, by sol-gel method prepare adsorption have the earthenware slab film of TiO2 particle with
Make film that there is photocatalysis, Chinese patent application CN201710280509.X discloses a kind of sewage treatment earthenware slab film
Separation membrane layer has obtained the strong sewage seperation film of antifouling property as the main component of film using graphene.Current separation
Film field requires the separation accuracy of earthenware slab film to further increase, and the intensity of seperation film itself is also to be improved to adapt to more
It is widely applied scene.
Summary of the invention
In order to solve the above technical problems, the present invention provides the ceramic membrane that a kind of separation accuracy is high, intensity is high.
The technical solution of the present invention is to provide a kind of filter plate ceramic membrane, composition includes the group of following parts by weight
Point: 60~80 parts of silicon carbide, 5~10 parts of silicon nitride, 5~8 parts of aluminium oxide, 3~6 parts of magnesia, 1~3 part of neodymia, polypropylene
0.1~1 part, 10~20 parts of styrene-acrylate emulsion, 0.1~0.5 part of polyvinyl alcohol of acid.
The thicknesses of layers of the filter plate ceramic membrane is 5~15 μm, and when film layer is excessively thin, filter hole can not regular landform
At, cause uniform pore diameter degree poor, filtering accuracy is very low, and when film layer is blocked up, although being capable of forming regular filter hole,
It is easily mutually to be overlapped by scanning electron microscopic observation filter hole, destroys the structure in whole duct, be equally unfavorable for improving filtering accuracy,
Therefore under the thicknesses of layers, pore size filter can be well controlled, and help to improve filtering accuracy.
The present invention also provides a kind of preparation methods of filter plate ceramic membrane, include the following steps:
S1. the 80wt% of above-mentioned raw materials (mass percent) is prepared into ceramic film support slurry, 20wt% prepares film layer
Slurry；
S2. silicon carbide, silicon nitride, aluminium oxide, magnesia, neodymia the preparation of ceramic film support slurry: are taken in proportion
15~20h of ball milling in ball mill is put into after mixing, polypropylene, styrene-acrylate emulsion are added afterwards, and polyvinyl alcohol continues
1~4h of ball milling；
S3. it the preparation of membrane layer pulp: is thrown after taking silicon carbide, silicon nitride, aluminium oxide, magnesia, neodymia to mix in proportion
Enter 24~36h of ball milling in ball mill, polypropylene, styrene-acrylate emulsion, polyvinyl alcohol, deionized water, continuation are added afterwards
1~4h of ball milling；
S4. the ceramic film support slurry in step S2 being made green body using the tape casting, green body spontaneously dries 24~
30h；
S5. sintered body, sintering parameter is to rise to 500 DEG C of 1~4h of heat preservation with 3~6 DEG C/min heating rate, with same
Heating rate rises to 1000 DEG C of 1~4h of heat preservation, finally rises to 1700~1850 DEG C with 10~20 DEG C/min heating rate, heat preservation 3
~6h；
S6. after green body is cooling, the membrane layer pulp prepared using cement-dipping method in billet surface impregnation steps S3, drying at room temperature
After be sintered, sintering parameter be 1~3 DEG C/min heating rate rise to 500 DEG C of 1~2h of heat preservation, risen to same heating rate
1700~1850 DEG C of 2~4h of heat preservation, it is cooling.
The solid content that the step S3 prepares resulting membrane layer pulp is respectively 30wt%, 50wt%, 60wt%, is used for
Green body repeatedly impregnates.
The step of step S6 green body soakage membrane slurry are as follows:
S61. the green body membrane layer pulp of solid content 60wt% is impregnated into 1h, it is dry；It repeats 1~2 time；
S62. the green body membrane layer pulp of solid content 50wt% is impregnated into 1h, it is dry；
S63. the green body membrane layer pulp of solid content 30wt% is impregnated into 1h, it is dry.
Green body cooling procedure is cooling with the rate of 2~4 DEG C/min in the step S6, and particle growth needs one in film layer
It fixes time, keeps certain rate of temperature fall that can control particle diameter, guarantee that film uniformity is good.
The advantages of the present invention: the main skeleton ingredient using silicon carbide, silicon nitride as ceramic membrane,
Grain diameter is reduced simultaneously by the uniformly grain diameter of each component by ball action when preparation, is conducive to form, and be sintered
The heating surface of each particle is approximate in the process, and close the guarantees heating of heating degree synchronizes, and when sintering, each particle growth speed approached simultaneously
Controllably；Each component forms eutectic liquids in film layer sintering process, and wherein silicon carbide and silicon nitride are in aluminium oxide, magnesia, neodymia
Under effect, forms particle overlapping in compact film and film layer and form cellular structure, porosity is aoxidized 40% or so
Aluminium, magnesia, neodymia can reduce the sintering temperature of ceramics, reduce energy consumption；Silicon nitride shape around silicon carbide when blank sintering
It is on the one hand connect with silicon-carbide particle at node, another aspect node interconnection itself constitutes the supplement of ceramic membrane
Support construction improves the intensity of silicon carbide support frame.
Specific embodiment
The invention will be further described With reference to embodiment.
Embodiment 1
The present invention provides a kind of filter plate ceramic membrane, and composition includes the component of following parts by weight: 60 parts of silicon carbide,
5 parts of silicon nitride, 5 parts of aluminium oxide, 3 parts of magnesia, 1 part of neodymia, 0.1 part of polyacrylic acid, styrene-acrylate emulsion 10
Part, 0.1 part of polyvinyl alcohol, thicknesses of layers is 5 μm.
The preparation method of above-mentioned filter plate ceramic membrane, includes the following steps:
S1. the 80wt% of above-mentioned raw materials (mass percent) is prepared into ceramic film support slurry, 20wt% prepares film layer
Slurry；
S2. silicon carbide, silicon nitride, aluminium oxide, magnesia, neodymia the preparation of ceramic film support slurry: are taken in proportion
Ball milling 15h in ball mill is put into after mixing, polypropylene, styrene-acrylate emulsion are added afterwards, and polyvinyl alcohol continues ball milling
1h；
S3. it the preparation of membrane layer pulp: is thrown after taking silicon carbide, silicon nitride, aluminium oxide, magnesia, neodymia to mix in proportion
Enter ball milling in ball mill and for 24 hours, polypropylene, styrene-acrylate emulsion, polyvinyl alcohol, deionized water, continuation ball milling is added afterwards
1h, obtained solid content is respectively that the membrane layer pulp of 30wt%, 50wt%, 60wt% are repeatedly impregnated for green body, obtained solid
The mass ratio of the membrane layer pulp of body content 30wt%, 50wt%, 60wt% is 2:1:2, and slurry is uniform after guaranteeing green body dipping
It is attached to surface；
S4. green body is made in the ceramic film support slurry in step S2 in a mold using the tape casting, green body is naturally dry
It is dry for 24 hours；
S5. sintered body, sintering parameter is to rise to 500 DEG C of heat preservation 2h with 3~6 DEG C/min heating rate, similarly to rise
Warm rate rises to 1000 DEG C of heat preservation 2h, finally rises to 1700~1850 DEG C with 10~20 DEG C/min heating rate, keeps the temperature 5h；
S6. it after cooling down green body with the rate of 2~4 DEG C/min, is prepared using cement-dipping method in billet surface impregnation steps S3
Membrane layer pulp, detailed process is to impregnate 1h with the membrane layer pulp of solid content 60wt%, dry, is repeated 1~2 time；Solid is used again
The membrane layer pulp of content 50wt% impregnates 1h, dry, finally impregnates 1h with the membrane layer pulp of solid content 30wt%, dry；Weight
The multiple higher membrane layer pulp of impregnation concentrations makes the tentatively abundant protective cover material of billet surface, uses impregnation concentrations again after dry
Slightly lower membrane layer pulp utilizes lower concentration difference and the billet surface of being formed with membrane layer pulp of billet surface film material concentration
Microcellular structure makes membrane layer pulp further be adsorbed to billet surface, at filling film layer defects, increases the complete of billet surface film layer
Degree and uniformity；
S7. it being sintered after drying at room temperature, sintering parameter is that 1~3 DEG C/min heating rate rises to 500 DEG C of 1~2h of heat preservation, with
Same heating rate rises to 1700~1850 DEG C of 2~4h of heat preservation, cooling.Flat ceramic membrane porosity obtained is 40%, by force
Degree is 15MPa, and filter hole aperture is 50~60nm.
Embodiment 2
The present invention provides a kind of filter plate ceramic membrane, and composition includes the component of following parts by weight: 80 parts of silicon carbide,
10 parts of silicon nitride, 8 parts of aluminium oxide, 6 parts of magnesia, 3 parts of neodymia, 1 part of polyacrylic acid, 20 parts of styrene-acrylate emulsion,
0.5 part of polyvinyl alcohol, thicknesses of layers is 15 μm.
The preparation method is the same as that of Example 1 for the present embodiment, flat ceramic membrane porosity obtained be 35%, intensity 18MPa,
Filter hole aperture is 50~60nm.
Embodiment 3
The present invention provides a kind of filter plate ceramic membrane, and composition includes the component of following parts by weight: 70 parts of silicon carbide,
8 parts of silicon nitride, 7 parts of aluminium oxide, 5 parts of magnesia, 2 parts of neodymia, 0.6 part of polyacrylic acid, styrene-acrylate emulsion 15
Part, 0.3 part of polyvinyl alcohol, thicknesses of layers is 10 μm.
The preparation method is the same as that of Example 1 for the present embodiment.Flat ceramic membrane porosity obtained be 32%, intensity 20MPa,
Filter hole aperture is 60~80nm.
Embodiment 4
The present invention provides a kind of filter plate ceramic membrane, and composition includes the component of following parts by weight: 75 parts of silicon carbide,
6 parts of silicon nitride, 6 parts of aluminium oxide, 4 parts of magnesia, 1.5 parts of neodymia, 0.8 part of polyacrylic acid, styrene-acrylate emulsion 18
Part, 0.2 part of polyvinyl alcohol, thicknesses of layers is 9 μm.
The preparation method is the same as that of Example 1 for the present embodiment.Flat ceramic membrane porosity obtained be 35%, intensity 19MPa,
Filter hole aperture is 50~60nm.
The present embodiments relate to the material arrived, reagent and experimental facilities, are to meet ceramic material unless otherwise instructed
The commercial product in field.
The above is merely a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, under the premise of not departing from core of the invention technology, improvements and modifications can also be made, these improvements and modifications are also answered
Belong to scope of patent protection of the invention.With any change in the comparable meaning and scope of claims of the present invention, all
It is considered as being included within the scope of the claims.
Claims (6)
1. a kind of filter plate ceramic membrane, composition includes the component of following parts by weight: 60~80 parts of silicon carbide, silicon nitride 5
~10 parts, 5~8 parts of aluminium oxide, 3~6 parts of magnesia, 1~3 part of neodymia, 0.1~1 part of polyacrylic acid, Styrene And Chloroalkyl Acrylates
10~20 parts of ester lotion, 0.1~0.5 part of polyvinyl alcohol.
2. filter plate ceramic membrane according to claim 1, which is characterized in that the film layer of the filter plate ceramic membrane is thick
Degree is 5~15 μm.
3. the preparation method of filter plate ceramic membrane described in claim 1, includes the following steps:
S1. the 80wt% of above-mentioned raw materials (mass percent) is prepared into ceramic film support slurry, 20wt% prepares membrane layer pulp；
S2. the preparation of ceramic film support slurry: silicon carbide, silicon nitride, aluminium oxide, magnesia, neodymia is taken to mix in proportion
15~20h of ball milling in ball mill is put into afterwards, polypropylene, styrene-acrylate emulsion are added afterwards, and polyvinyl alcohol continues ball milling 1
~4h；
S3. the preparation of membrane layer pulp: ball is put into after taking silicon carbide, silicon nitride, aluminium oxide, magnesia, neodymia to mix in proportion
Polypropylene, styrene-acrylate emulsion, polyvinyl alcohol, deionized water, continuation ball milling is added in 24~36h of ball milling in grinding machine afterwards
1~4h；
S4. green body is made in the ceramic film support slurry in step S2 using the tape casting, green body spontaneously dries 24~30h；
S5. sintered body, sintering parameter is to rise to 500 DEG C of 1~4h of heat preservation with 3~6 DEG C/min heating rate, similarly to heat up
Rate rises to 1000 DEG C of 1~4h of heat preservation, finally rises to 1700~1850 DEG C with 10~20 DEG C/min heating rate, keeps the temperature 3~6h；
S6. after green body is cooling, the membrane layer pulp prepared using cement-dipping method in billet surface impregnation steps S3 is burnt after drying at room temperature
Knot, sintering parameter are that 1~3 DEG C/min heating rate rises to 500 DEG C of 1~2h of heat preservation, 1700 are risen to same heating rate~
1850 DEG C of 2~4h of heat preservation, it is cooling.
4. the preparation method of filter plate ceramic membrane according to claim 3, which is characterized in that the step S3 prepares institute
The solid content of the membrane layer pulp obtained is respectively 30wt%, 50wt%, 60wt%, is repeatedly impregnated for green body.
5. the preparation method of filter plate ceramic membrane according to claim 4, which is characterized in that the step S6 green body leaching
The step of stain membrane layer pulp are as follows:
S61. the green body membrane layer pulp of solid content 60wt% is impregnated into 1h, it is dry；It repeats 1~2 time；
S62. the green body membrane layer pulp of solid content 50wt% is impregnated into 1h, it is dry；
S63. the green body membrane layer pulp of solid content 30wt% is impregnated into 1h, it is dry.
6. the preparation method of filter plate ceramic membrane according to claim 3, which is characterized in that green body in the step S6
Cooling procedure is cooling with the rate of 2~4 DEG C/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110698215A (en) * | 2019-10-29 | 2020-01-17 | 中国科学院上海硅酸盐研究所苏州研究院 | High-temperature-resistant corrosion-resistant reaction-sintered silicon carbide film support and preparation method thereof |
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| CN110698215A (en) * | 2019-10-29 | 2020-01-17 | 中国科学院上海硅酸盐研究所苏州研究院 | High-temperature-resistant corrosion-resistant reaction-sintered silicon carbide film support and preparation method thereof |
| CN111567893A (en) * | 2020-04-08 | 2020-08-25 | 深圳麦克韦尔科技有限公司 | Heating element, preparation method thereof and heating non-combustible aerosol forming device |
| CN111470869A (en) * | 2020-05-08 | 2020-07-31 | 武汉工程大学 | Preparation method of separation membrane based on high-solid-content silicon carbide slurry |
| CN111533572A (en) * | 2020-05-08 | 2020-08-14 | 武汉工程大学 | Preparation method of porous silicon carbide ceramic support |
| CN111533572B (en) * | 2020-05-08 | 2022-03-15 | 武汉工程大学 | Preparation method of porous silicon carbide ceramic support |
| JP7099739B2 (en) | 2020-05-08 | 2022-07-12 | 武漢工程大学 | Method for manufacturing porous silicon carbide ceramic carrier |
| CN111470869B (en) * | 2020-05-08 | 2022-07-19 | 武汉工程大学 | Preparation method of separation membrane based on high-solid-content silicon carbide slurry |
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