CN109400203A - A kind of preparation method of graphene inorganic porous ceramic film - Google Patents
A kind of preparation method of graphene inorganic porous ceramic film Download PDFInfo
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
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Abstract
The present invention relates to a kind of preparation methods of graphene inorganic porous ceramic film, comprising the following steps: mixes graphene powder with deionized water, chitosan, micro-ceramic powder, nanoscale sintering aid, settles, filters, drying and form modified graphene inorganic particle；Modified graphene inorganic particle, adhesive are mixed to get premix ceramic material, then carry out pugging, extruded ceramic film green dries, sinters graphene inorganic porous ceramic film into.Graphene ceramic membrane prepared by the present invention, simple process, the mechanical strength of ceramic membrane can effectively be improved, especially in toughening intensity, so that its stable operation in harsher strong acid, highly basic, the environment big across the temperature difference, and greatly reduce fracture rate caused by ceramic membranous system shakes because of equipment in operation.Preparation method of the invention has many advantages, such as that process flow is simple, production cost is low, environmental-friendly, production serialization, has a possibility that industrialized production.
Description
Technical field
The invention belongs to environmental protection technical field, in particular to inorganic field of membrane preparation, specially a kind of graphene without
The preparation method of machine porous ceramic film.
Background technique
Ceramic membrane (ceramic membrane) is also known as inorganic ceramic membrane, is to be prepared with inorganic ceramic material through special process
And the anisotropic membrane formed.Ceramic membrane tube wall gathers micropore, under pressure, former according within the scope of certain membrane aperture
Feed liquid flows in membrane tube or on the outside of film, and water, inorganic salts, small-molecule substance (or liquid) penetrate film, suspended matter, glue and microorganism
Equal macromolecular substances (or solid) is rejected by, to reach the purpose of separation, concentration, purifying and environmental protection.Ceramic membrane, which has, to be divided
From high-efficient, effect stability, chemical stability is good, acid and alkali-resistance, organic solvent-resistant, resistance to bacterium, high temperature resistant, antipollution, mechanical strength
Numerous advantages such as high, regenerability is good, separation process is simple, low energy consumption, simple and convenient operation and maintenance, long service life, have succeeded
Applied to various fields such as food, beverage, the processing of plant (medicine) object depth, biological medicine, fermentation, fine chemistry industries, it can be used for technique mistake
Separation, clarification, purifying, concentration, degerming, desalination in journey etc.
Graphene is most thin most hard nano material in the world, and single-layer graphene thickness is only 0.34nm and nearly transparent,
Thermal coefficient is up to 5300W/ (mK), and electron mobility is more than 15000cm at room temperature2/ (Vs), specific surface area reach 2965m2/
G, tensile strength about 130GPa, elasticity modulus 1Tpa.Graphene uniform is mixed with the ceramic powder raw material such as aluminium oxide, is being sintered
In the process, graphene solves the problems, such as that sintering is difficult in traditional ceramics film, pore-forming is not easy to control, energy consumption is high, is made
Graphene ceramic membrane, there is that aperture is easy to control and separative efficiency is high, chemical stability is good, acid and alkali-resistance, organic solvent-resistant, resistance to bacterium, resistance to
Numerous advantages such as high temperature, high mechanical strength, regenerability are good, low energy consumption, long service life.
Currently, the research that related graphene imported into inorganic ceramic membrane is less.China Patent No. 200510075913.0 is public
A kind of manufacturing method of ceramic membrane has been opened, has contained Ca-Ti ore type collosol and gel raw material and more this method comprises: being formed on matrix
The process of the former material Material of core metal complex raw material, and make the process of above-mentioned former material Material crystallization.Comprising passing through
The process for crystallizing former material Material 20 and forming ceramic membrane 30, former material Material 20 contain type difference with the state being mixed
Raw material, diverse raw material each other the crystal growth condition in the crystallization of raw material and mechanism of crystal growth at least one
There are mutually different relationships for side.Manufacturing method according to the invention can improve the configuration of surface of ceramic membrane.The patent is not
Foot place is that sintering aid is numerous, and in actual high temperature sintering, crystallisation procedure is uncontrollable.China Patent No.
201510177549.2 disclose a kind of preparation method of water process tubular membrane comprising following steps: (1) preparation support
Body: it using alumina powder as aggregate, is added after silicon carbide whisker, pore creating material, sintering aid and water are mixed into slurry and grinds, then to slurry
Then plasticizer and water regrinding is added in ageing, drying, then by pipe die molding, drying, be then sintered, clean, obtain
Tubular type supporter；(2) it prepares colloidal sol: ground aluminium isopropoxide being added in the deionized water of heat and carry out magnetic agitation, then divided
It criticizes and nitric acid is added, then stirring to solution clear is added dispersing agent and defoaming agent stirs evenly, obtains colloidal sol, then be aged
Colloidal sol；(3) it coats: support external surface being pasted into one layer of sealing film, then supporter is immersed in the colloidal sol being aged, then up
Colloidal sol liquid level is lifted out, supporter inner surface is made to coat one layer of liquid film；(4) gelation: sealing film is removed, then liquid will be coated with
The supporter of film is placed in.Continue to form a film in atmosphere containing vapor, liquid film is made to be transformed into gel mould；(5) it cleans, is dry
It is dry: the outer surface of cleaning tubular type supporter, it is then dry to gel mould using classification seasoning；(6) it is sintered: to dry gel
Film sintering.The patent is disadvantageous in that complex process, the poor controllability in actual industrial volume production, be easy to cause quality unstable
Determine, ceramic membrane narrow application range at high cost, while preparing, acid-proof alkaline is general.
Graphene ceramic membrane prepared by the present invention, simple process can effectively improve the mechanical strength of ceramic membrane, especially
It is in toughening intensity, so that its stable operation in harsher strong acid, highly basic, the environment big across the temperature difference, and significantly
Reduce fracture rate caused by ceramic membranous system shakes because of equipment in operation.Preparation method of the invention has process flow letter
Single, the advantages that production cost is low, environmental-friendly, production serialization, has a possibility that industrialized production.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of graphene inorganic in view of the above shortcomings of the prior art
The preparation method of porous ceramic film, technical process is simple, can industrial volume production, high-efficiency environment friendly.
In order to solve the above technical problems, solution of the invention is:
A kind of graphene inorganic porous ceramic film and preparation method thereof, specific steps are as follows:
Step (1): the preparation of modified graphene inorganic particle
(a) graphene powder and deionized water are added in blender, stirring slurry revolving speed is set as under 300-500r/min
It rotates forward 30 minutes, inverts 30 minutes later, then by Nano-meter SiO_22It is added in blender, rotates forward 30 minutes, be slow added into shell
Glycan, micro-ceramic powder and nanoscale sintering aid etc. are added, and rotate forward 30 minutes, obtain the mixing of modified graphene inorganic particle
Slurry, wherein nanoscale agglutinant forms compound ligand mode with micro-ceramic powder and is added together with chitosan again；
(b) slurry is placed in sedimentation cylinder, and after filtering supernatant, drying obtains modified graphene inorganic particle.
The composition of raw materials is (following alleged number is by weight): graphene powder is 0.1-1.2 parts, ceramic powder
Body is 50-99.5 parts, and sintering aid is 0.1-0.8 parts, Nano-meter SiO_220.1-0.8 parts, chitosan is 0.1-1 parts
Step (2): mixing, pugging
(a) modified graphene inorganic particle, adhesive are added in blender, are mixed 20-60 minutes, obtain premix ceramics
Pug；(b) pug is put into pug mill, is recycled 2 to 3 times.
The composition of raw materials is (following alleged number is by weight): modified graphene inorganic particle is 98-99.5
Part, adhesive is 0.5-1 parts.
Step (3): extrusion molding
Pug is put into extruder, by selecting different molds, extruded ceramic film green, then by green batch
Amount is put into baking oven, is dried.
Step (4): sintering
Green is put into high temperature sintering kiln, the heating curve program of kiln is set, maximum temperature is controlled in 1650-
2150 DEG C, soaking time 80-120min, sinter green into graphene inorganic porous ceramic film.
The micro-ceramic powder is that aluminium oxide, zirconium oxide or alumina-zirconia compound mixture, wherein aoxidizing
Alumina powder is 50-99.5 parts in aluminium/zirconium oxide compounding mixture, and (the above alleged number is all for 50-99.5 parts of Zirconium powder
It is by weight).
The nanoscale sintering aid is nanometer magnesia powder, nano chromium oxide powder.
Described adhesive is nanometer silicon carbide, nano-titanium dioxide, polysulfones (PSF), polyether sulfone (PES), polyacrylonitrile
(PAN) and one of polyetherimide (PEI).
The graphene is preferably the graphene of mechanical stripping method preparation.
The features of the present invention and the utility model has the advantages that
(1) graphene of mechanical stripping method is used, the graphene crystal structure is complete, and defect is few, itself has excellent
Elasticity modulus, tensile strength；(2) the graphene surface functional group added is few, and monomer chemistries have good stability, in sintering process
The crystal boundary graphitization of middle ceramics easily controls, and then greatly reduces the use of traditional ceramics film sintering aid, improves sintering
The product qualification rate of technique, while the maximum holding temperature of sintering is reduced, energy consumption is greatly reduced, the cost of ceramic membrane is reduced；
(3) technique provided by the invention and formula can be such that the ceramic powders raw material such as graphene and aluminium oxide is sufficiently mixed, sintered
Cheng Zhong, graphene can be nano-modified to ceramic membrane progress, and graphene uniform is distributed in ceramic crystal phase, so that graphene is ceramic
Film has extremely strong comprehensive mechanical performance, while the ceramic membrane to insulate originally being made to obtain certain electrical property, so that initiative allows
Ceramic membrane obtains the expansion performance of the traditional ceramics film such as charge, bio-compatibility expectation；(4) graphene specific surface area is high, makes
Hole ability is strong, solves the problems, such as that traditional inorganic ceramic membrane is added excessive pore creating material and ceramic membrane mechanical strength is caused to decline；
(5) preparation method of graphene composite ceramic film provided by the invention is with process flow is simple, production cost is low, environment is friendly
Good, production can serialization the advantages that, have a possibility that industrialized production.
Specific embodiment
In order to better understand the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but in the present invention
Appearance is not limited solely to specific embodiment below.
Embodiment 1
Alleged number is by weight below.
Step (1): the preparation of modified graphene inorganic particle
(a) 0.1 part of graphene powder and deionized water are added in blender, stirring slurry revolving speed is set as under 300r/min
It rotates forward 30 minutes, inverts 30 minutes later, then by 0.1 part of Nano-meter SiO_22It is added in blender, rotates forward 30 minutes.By 0.1 part
Nanoscale magnesium forms compound ligand mode with 50 parts of micron grade aluminum oxides and is added together with 0.1 part of chitosan again；Rotate forward 30 points
Clock obtains modified graphene inorganic particle mixed slurry；
(b) slurry is placed in sedimentation cylinder, and after filtering supernatant, drying obtains modified graphene inorganic particle.
Step (2): mixing, pugging
(a) 98 parts of modified graphene inorganic particles, 0.5 part of nano-titanium dioxide are added in blender, are mixed 30 minutes,
Obtain premix ceramic material；(b) pug is put into pug mill, is recycled 2 to 3 times.
Step (3): extrusion molding
Pug is put into extruder, extruded ceramic film green, green batch is then put into baking oven, is dried
It is dry.
Step (4): sintering
Green is put into high temperature sintering kiln, the heating curve program of kiln is set, maximum temperature is controlled 1650
DEG C, soaking time 120min sinters green into graphene inorganic porous ceramic film.
Embodiment 2
Alleged number is by weight below.
Step (1): the preparation of modified graphene inorganic particle
(a) 0.5 part of graphene powder and deionized water are added in blender, stirring slurry revolving speed is set as under 300r/min
It rotates forward 30 minutes, inverts 30 minutes later, then by 0.3 part of Nano-meter SiO_22It is added in blender, rotates forward 30 minutes.By 0.4 part
Nano chromium oxide powder forms compound ligand mode with 75 parts of micron grade aluminum oxides and is added together with 0.5 part of chitosan again；Rotate forward 30
Minute, obtain modified graphene inorganic particle mixed slurry；
(b) slurry is placed in sedimentation cylinder, and after filtering supernatant, drying obtains modified graphene inorganic particle.
Step (2): mixing, pugging
(a) 98 parts of modified graphene inorganic particles, 1 part of nano-titanium dioxide are added in blender, 20-60 points of mixing
Clock obtains premix ceramic material；(b) pug is put into pug mill, is recycled 2 to 3 times.
Step (3): extrusion molding
Pug is put into extruder, extruded ceramic film green, green batch is then put into baking oven, is dried
It is dry.
Step (4): sintering
Green is put into high temperature sintering kiln, the heating curve program of kiln is set, maximum temperature is controlled 2150
DEG C, soaking time 80min sinters green into graphene inorganic porous ceramic film.
Embodiment 3
Alleged number is by weight below.
Step (1): the preparation of modified graphene inorganic particle
(a) 1 part of graphene powder and deionized water are added in blender, stirring slurry revolving speed is set as under 300r/min just
Turn 30 minutes, inverts 30 minutes later, then by 0.6 part of Nano-meter SiO_22It is added in blender, rotates forward 30 minutes.0.4 part is received
Rice chromium oxide powder compounds mixture (wherein 50 parts of aluminium oxide, zirconium oxide 49.5 with 99.5 parts of micron order alumina-zirconias
Part) formed compound ligand mode be added together with 1 part of chitosan again；It rotates forward 30 minutes, obtains the mixing of modified graphene inorganic particle
Slurry；
(b) slurry is placed in sedimentation cylinder, and after filtering supernatant, drying obtains modified graphene inorganic particle.
Step (2): mixing, pugging
(a) 98 parts of modified graphene inorganic particles, 0.5 part of nanometer silicon carbide are added in blender, mix 40 minutes, obtains
To premix ceramic material；(b) pug is put into pug mill, is recycled 2 to 3 times.
Step (3): extrusion molding
Pug is put into extruder, extruded ceramic film green, green batch is then put into baking oven, is dried
It is dry.
Step (4): sintering
Green is put into high temperature sintering kiln, the heating curve program of kiln is set, maximum temperature is controlled 2150
DEG C, soaking time 120min sinters green into graphene inorganic porous ceramic film.
Embodiment 4
Alleged number is by weight below.
Step (1): the preparation of modified graphene inorganic particle
(a) 1 part of graphene powder and deionized water are added in blender, stirring slurry revolving speed is set as under 300r/min just
Turn 30 minutes, inverts 30 minutes later, then by 0.8 part of Nano-meter SiO_22It is added in blender, rotates forward 30 minutes.0.4 part is received
Rice magnesium oxide powder compounds mixture (wherein 20 parts of aluminium oxide, zirconium oxide 79.5 with 99.5 parts of micron order alumina-zirconias
Part) formed compound ligand mode be added together with 1 part of chitosan again；It rotates forward 30 minutes, obtains the mixing of modified graphene inorganic particle
Slurry；
(b) slurry is placed in sedimentation cylinder, and after filtering supernatant, drying obtains modified graphene inorganic particle.
Step (2): mixing, pugging
(a) 99 parts of modified graphene inorganic particles, 0.5 part of nano polypropylene nitrile are added in blender, are mixed 60 minutes,
Obtain premix ceramic material；(b) pug is put into pug mill, is recycled 2 to 3 times.
Step (3): extrusion molding
Pug is put into extruder, extruded ceramic film green, green batch is then put into baking oven, is dried
It is dry.
Step (4): sintering
Green is put into high temperature sintering kiln, the heating curve program of kiln is set, maximum temperature is controlled 2150
DEG C, soaking time 120min sinters green into graphene inorganic porous ceramic film.
The above selected embodiment is typical embodiments, and above description is merely used to help understand method of the invention
And its core concept.It should be pointed out that for those skilled in the art, before not departing from the principle of the invention
It puts, can be with several improvements and modifications are made to the present invention, these improvement and modification also fall into the guarantor of the claims in the present invention
It protects in range.
Claims (5)
1. a kind of graphene inorganic porous ceramic film and preparation method thereof, it is characterised in that specific steps are as follows:
Step (1): the preparation of modified graphene inorganic particle
(a) graphene powder and deionized water are added in blender, stirring slurry revolving speed is set as rotating forward under 300-500r/min
It 30 minutes, inverts 30 minutes later, then by Nano-meter SiO_22It is added in blender, rotates forward 30 minutes, be slow added into micron order
Ceramic powder and nanoscale sintering aid, chitosan etc. are added, and rotate forward 30 minutes, obtain modified graphene inorganic particle mixing slurry
Material；Wherein nanoscale agglutinant forms compound ligand mode with micro-ceramic powder and is added together with chitosan again；
(b) slurry is placed in sedimentation cylinder, and after filtering supernatant, drying obtains modified graphene inorganic particle；
The composition of raw materials is (following alleged number is by weight): graphene powder is 0.1-1.2 parts, and ceramic powder is
50-99.5 parts, sintering aid is 0.1-0.8 parts, Nano-meter SiO_220.1-0.8 parts, chitosan is 0.1-1 parts；
Step (2): mixing, pugging
(a) modified graphene inorganic particle, adhesive are added in blender, mix 20-60 minutes, obtains premixing ceramic mud
Material；(b) pug is put into pug mill, is recycled 2 to 3 times.
The composition of raw materials is (following alleged number is by weight): modified graphene inorganic particle is 98-99.5 parts, is glued
Mixture is 0.5-1 parts；
Step (3): extrusion molding
Pug is put into extruder, by selecting different molds, then extruded ceramic film green puts green batch
Enter baking oven, is dried；
Step (4): sintering
Green is put into high temperature sintering kiln, the heating curve program of kiln is set, maximum temperature is controlled in 1650-2150
DEG C, soaking time 80-120min sinters green into graphene inorganic porous ceramic film.
2. a kind of graphene inorganic porous ceramic film as described in claim 1 and preparation method thereof, it is characterised in that described micro-
Meter level ceramic powder is that aluminium oxide, zirconium oxide or alumina-zirconia compound mixture, and wherein alumina-zirconia compounding is mixed
Closing alumina powder in object is 50-99.5 parts, 50-99.5 parts of Zirconium powder (the above alleged number is by weight).
3. a kind of graphene inorganic porous ceramic film as described in claim 1 and preparation method thereof, it is characterised in that described to receive
Meter level sintering aid is nanometer magnesia powder, nano chromium oxide powder.
4. a kind of graphene inorganic porous ceramic film as described in claim 1 and preparation method thereof, it is characterised in that described viscous
Mixture is nanometer silicon carbide, nano-titanium dioxide, polysulfones (PSF), polyether sulfone (PES), polyacrylonitrile (PAN) and polyetherimide
One of (PEI).
5. a kind of graphene inorganic porous ceramic film as described in claim 1 and preparation method thereof, it is characterised in that the stone
Black alkene is the graphene of mechanical stripping method preparation.
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| CN115557778A (en) * | 2022-10-24 | 2023-01-03 | 江苏天合绿色氢能源科技有限公司 | Ceramic composition, microfiltration ceramic membrane, and preparation method and application thereof |
| CN116477923A (en) * | 2023-03-22 | 2023-07-25 | 雅安沃克林环保科技有限公司 | Method for preparing ceramic connecting plate by utilizing ceramic membrane waste and ceramic connecting plate |
| CN116477923B (en) * | 2023-03-22 | 2024-04-05 | 雅安沃克林环保科技有限公司 | Method for preparing ceramic connecting plate by utilizing ceramic membrane waste and ceramic connecting plate |
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