CN109721339A - A method of preparing the Ceramic Hollow Fiber based on nanoscale composition granule - Google Patents
A method of preparing the Ceramic Hollow Fiber based on nanoscale composition granule Download PDFInfo
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- CN109721339A CN109721339A CN201910115693.1A CN201910115693A CN109721339A CN 109721339 A CN109721339 A CN 109721339A CN 201910115693 A CN201910115693 A CN 201910115693A CN 109721339 A CN109721339 A CN 109721339A
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Abstract
The present invention relates to the methods of Ceramic Hollow Fiber of the preparation based on nanoscale composition granule, it discloses and batch ceramic and its manufacturing method is provided on nano-scale particle, by converting nanosize metal oxide with hydroxycarboxylic acid, carbide, nitride or sulfide powder, at least one solvent and acrylate is used to mix manufacture ceramic block and/or methacrylate with ceramic block as polymer adhesive, metal oxide, carbide, the partial size of nitride or sulfide powder is 1-50nm, and the solid content of ceramic masses is greater than 30%；It is added into ceramic block carbon-based, organic or inorganic component is as expendable material, in an amount of from 5-20wt%；Ceramic block is squeezed or is spun to doughnut blank；By using radial starter polymeric acrylate and/or methacrylate adhesives；It is sintered blank, forms outer diameter 100um, fiber of the aperture between 0.5-100nm, the doughnut produced in this way should be porous respectively according to application field or sinter into close to theoretical density.
Description
Technical field
It is specially a kind of to prepare the present invention relates to the method for Ceramic Hollow Fiber of the preparation based on nanoscale composition granule
The method of Ceramic Hollow Fiber based on nanoscale composition granule.
Background technique
Ceramic fibre is realizing more and more industrial significances, wherein the entire ceramic fibre of especially aluminium oxide is
Can get on the market, therefore, 3M, three wells, Sumitomo and Toyota Company provide price 400 to 1800 dollars/kilograms it
Between continuous aluminium oxide ceramics, short ceramic fibre of the length within the scope of 1um have lesser industrial significance, due to ceramic fibre
Lung may be sucked, therefore these fibers may be processed no longer in Germany, the new development in Ceramic Hollow Fiber field becomes
Gesture is being shown up prominently, and Ceramic Hollow Fiber establishes Ceramic Hollow Fiber principle in all fields that Whole fiber has been established, and is gone forward side by side
One step develops other and segments market, although however, Ceramic Hollow Fiber is not yet commercialized, but the reality of many research institutions
The theme of development, compared with Whole fiber, doughnut has bigger bending strength and higher insulating coefficient, with lower material
Expect dosage (about 40-60% weight) together, while saving the weight of same volume, in addition, hollow body can be cooling from inside,
Such as heat, internal material etc. can easily be transported to outside, and the most important application field of Ceramic Hollow Fiber is metal, gather
Close object and ceramic sheath, man-made organ, optical fiber, ceramic membrane, the solid electrolyte of (SOFC) fuel cell, organizational project, weaving
It industry and manufactures extremely light, ceramic structural elements resistant to high temperature and can purposefully radiate such as thermal insulation board or braking system, and it is flat
Face structure is compared, and doughnut is structure that is three-dimensional and also generating rotational symmetry, this also allows to be permitted in microsystems technology
Mostly flexibly used in application.
In order to realize the ceramic of compact doughnut with small outer diameter and inner diameter and with various desirably economical
Material realize, there are two types of possibility, or use template, be removed in second step and thus generation transitional fibre is right
And using very small ceramic particle, it may then pass through conventional shaping method of ceramics such as electrophoresis, squeeze out or tape casting will
Doughnut is made in it, however manufactures Ceramic Hollow Fiber or prepare entire doughnut from nano particle or must make
The doughnut with layer structure is made, during the multilayer system that calcining is made of porous carrier and layer, nano-particle layer will
It always falls off in the interface with macropore carrier, because Temperature Treatment causes the rear crystallization of nano particle, this triggers strong receipts
Contracting and serious pressure, this part can destroy this part, and the preparation for carrying Ceramic Hollow Fiber has very high industrial significance, nanometer
The work of particle preparation Ceramic Hollow Fiber is also new technique.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of ceramic hollows prepared based on nanoscale composition granule
The method of fiber, the content of powder height of the solid content of nano particle and therefore batch of material by ceramics extrusion in can be produced
Hollow fiber, the doughnut manufactured in this way simultaneously allow them to be transformed into Ceramic Hollow Fiber in downstream process, in this way
The doughnut of production should be porous respectively according to application field or sinter into close to theoretical density.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs: a kind of to prepare based on nanoscale
The method of the Ceramic Hollow Fiber of composition granule, including hydroxycarboxylic acid, nanometer grade powder, solvent, polymer adhesive, device for spinning
With radial starter.
Preferably, the nanometer grade powder includes the unstable zirconium oxide of aluminium oxide, zirconium oxide, yttrium, titanium oxide, silicon carbide
With tungsten carbide/or silicon nitride, batch of material of the invention preferably comprises nano-scale particle, regardless of whether processing Si, Al, B, Zn, Zr,
The oxide of Cd, Ti, Ce, Sn, In, oxide hydrate, chalcogenide, nitride or carbide, La, Fe, Cu, Ta, Nb,
V, Mo or W, particularly preferred oxide, preferred nano grade inorganic solid granulates are aluminium oxide, zirconium oxide, titanium oxide, silicon carbide,
Tungsten carbide and silicon nitride.
Preferably, the hydroxycarboxylic acid is selected from trioxa capric acid and dioctyl enanthic acid, after shaping by using freedom
Base initiator can be radiated for example, by UV or is crosslinked by hot method, so that required polymer is formed, it is according to the present invention
Component in batch of material.Here all acrylate commercially found and methacrylate compound are all suitable, but excellent
Select BASF with those of Lucin and Laromer tag sale.
Preferably, the solvent is water, ethylene glycol, propylene glycol, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether and second two
The mixture of alcohol and diethylene glycol monobutyl ether.
Preferably, the polymer adhesive is cellulose, methylcellulose, ethyl cellulose, polyvinyl alcohol, carboxymethyl
Sodium cellulosate and polyacrylate/or polymethacrylates.
S1, preferably batch of material contain nano-scale particle, regardless of whether processing Si, Al, B, Zn, Zr, Cd, Ti, Ce, Sn, In's
Oxide, oxide hydrate, chalcogenide, nitride or carbide, La, Fe, Cu, Ta, Nb, V, Mo or W, particularly preferred oxygen
Compound, preferred nano grade inorganic solid granulates are aluminium oxide, zirconium oxide, titanium oxide, silicon carbide, tungsten carbide and silicon nitride, are somebody's turn to do
The average grain diameter of inorganic particle contained in batch of material is usually 1 to 300nm or 1 to 100nm, preferably 5 to 50nm, particularly preferably
To 20nm, primary granule can also exist with agglomerated form, but preferably not agglomeration or substantially not agglomeration.
The selection and configuration of S2, polymer adhesive, using any thermoplastic polymer, especially commonly used in extrusion
Those, such as polyethylene, bialkyl ortho phthalate (repefral, diethyl phthalate, phthalic acid
Dipropyl, dibutyl phthalate), polypropylene and poly- 1- butane, poly- methyl (methyl) acrylate, polyacrylonitrile, polyphenyl
Ethylene and polyvinyl alcohol, polyamide, polyester, poly- acetic acid esters, polycarbonate, linear polyester and corresponding copolymer, such as ethylene-
Vinyl acetate (EVA) copolymer and biopolymer such as cellulose and ancient Chinese name for Venus etc., wherein polyacrylate, poly- methyl-prop
Olefin(e) acid ester, cellulose and keel glue be it is preferred, thermoplastic polymer or two or more thermoplastic polymers can be used
Mixture, using acrylate and methacrylate, after shaping by using radical initiator, for example, by UV spoke
It penetrates or is crosslinked by hot method, form required polymer.
S3, initial powder is mixed with organic bond, wherein at least one polymer adhesive and at least one hydroxyl
Carboxylic acid and at least one solvent.
S4, in conventional mixing and kneader device, nanometer grade powder and polymer, oxa- carboxylic acid and solvent or solvent are mixed
Object mixing is closed, carries out enough time using kneader, double screw extruder, heavy roll squeezer, three roller looms or mortar grinder
Mixing and kneading, obtain uniform mixture.
S5, sintering blank.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
The present embodiment 1:
The processing of the stable zirconium oxide of nanoscale yttrium carries out in commercially available aggregated mixed device, and wherein content of powder is set as
72% (by mass) provides the solvent mixture of the 1:1 ratio of 300g ethylene glycol and ethylene glycol monobutyl ether, into the mixture
The 700g nanoscale zirconia modified with dioctyl-acetic acid is added, be further added 140g acrylate-based adhesives system with
And after radical initiator, by mixture homogenization.Then by the thickener so prepared silk-screen printing under stress, in ceramics or gold
Belong to and generate flatness layer in substrate, using macking technique and be exposed to ultraviolet radiation, polymerization generates extremely fine structure, can be with
Unpolymerized region is removed by washing.
Embodiment 2:
The processing oxide of nanometer Yt doped zirconium is by squeezing commercially available aggregate blender, and powder content is set as 72%
(by mass), 300 grams of solvent mixture ethylene glycol and butyl carbitol pyrethroids 1:1 provide the ratio of this mixture and are
700 grams of nanoscales are newly-increased with dinitro enanthic acid modified zirconia, in further 140 grams of acrylate-based adhesives systems of addition
(drawing section Meier, BASF) and free radical starter homogenize mixture, then by the paste being prepared ceramics
Hollow extrusion deep processing fiber；Ceramic block is Qiao by a kind of outer diameter sapphire nozzle for being 100 and an inside center
Wood, 7 such nozzles are mounted on steelframe in total, and are extruded under the pressure of 10 to 30 megapascal, personal finally with unlimited
Variable reel picks up fiber revolving speed, and line speed is 5 meters per hour, and the microporous fibre after crosslinking has 70 microns of outer diameter, internal diameter
It 50 microns, is cut from the continuous fiber of this 20 centimeter length of root, wherein being nailed together or weave in, 1050
At a temperature of DEG C, organic principle and 2 hours Ceramic Hollow Fibers of sintering or Ceramic Hollow Fiber net, the outer diameter of Ceramic Hollow Fiber are
56 microns, internal diameter is 40 microns, density 97%.
Embodiment 3:
The processing oxide of nanometer Yt doped zirconium is by squeezing commercially available aggregate blender, and powder content is set as 72%
(by mass), 300 grams of solvent mixture ethylene glycol and butyl carbitol pyrethroids 1:1 provide the ratio of this mixture and are
700 grams of nanoscales are newly-increased with dinitro enanthic acid modified zirconia, in further 140 grams of acrylate-based adhesives systems of addition
(drawing section Meier, BASF) and free radical starter homogenize mixture, then by the paste being prepared ceramics
Hollow extrusion deep processing fiber；Ceramic block is Qiao by a kind of outer diameter sapphire nozzle for being 100 and an inside center
Wood, 7 such nozzles are mounted on steelframe in total, and are extruded under the pressure of 10 to 30 megapascal, personal finally with unlimited
Variable reel picks up fiber revolving speed, and line speed is 5 meters per hour, and the microporous fibre after crosslinking has 70 microns of outer diameter, internal diameter
It 50 microns, is cut from the continuous fiber of this 20 centimeter length of root, wherein being nailed together or weave in, 1050
At a temperature of DEG C, organic principle and 2 hours Ceramic Hollow Fibers of sintering or Ceramic Hollow Fiber net, the outer diameter of Ceramic Hollow Fiber are
56 microns, internal diameter is 40 microns, and 65g sacrifice active carbon is added in batch of material density 97%, is sintered 2 hours at 1050 DEG C
Afterwards, porous hollow fiber, porosity 35%, average pore size 5nm are obtained.
Embodiment 4
It is carried out in commercially available aggregate mixer by squeezing out processing alumina in Nano level, wherein content of powder is set as
71% (by mass) provides the solvent mixture of the 1:1 ratio of 300g ethylene glycol and ethylene glycol monobutyl ether, into the mixture
The 700g nanoscale zirconia modified with dioctyl-acetic acid is added, be further added 140g acrylate-based adhesives system with
And after radical initiator, then the thickener being prepared is further processed into ceramics by mixture homogenization by squeezing out
Hollow fiber, for this purpose, ceramic mass is conveyed by sapphire nozzle, external nozzles diameter is 100um, and inside is the center heart
Axis, in these nozzles in total 7 be mounted in steel frame and squeezed out under 10 to 30MPa pressure, finally have it is unlimited
Single fiber is picked up on the spool of speed variable, centerline velocities are 5 meters per second, after crosslinking, and the outer diameter of micro- doughnut is 70
Micron, internal diameter are 50 microns, and 20 centimetres of length is cut from this continuous fiber, they are nailed together or is interweaved one
It rises, after discharging organic component and being sintered 2 hours at 950 DEG C, obtains Ceramic Hollow Fiber or reticulated ceramic doughnut, make pottery
The outer diameter of porcelain doughnut is 60 microns, and internal diameter is 45 microns, and density is the 98% of theoretical value.
Embodiment 5:
The processing of nanoscale zirconia is carried out by squeezing out in commercially available aggregated mixed device, and wherein content of powder is set as
72% (by mass) provides the solvent mixture of the 1:1 ratio of 300g ethylene glycol and ethylene glycol monobutyl ether, into the mixture
The 700g nanoscale zirconia modified with dioctyl-acetic acid is added, 140g acrylate-based adhesives system is further being added
After (Lacromer, BASF) and radical initiator, by mixture homogenization, then by squeezing out Ceramic Hollow Fiber into one
The paste that step processing is so prepared, for this purpose, ceramic mass is conveyed by sapphire nozzle, external nozzles diameter is 100
Micron, it is internal centered on mandrel, in these nozzles in total 7 be mounted in steel frame, and under 10 to 30MPa pressure
It squeezes out, finally picks up single fiber on the spool with infinite variable revolving speed, after crosslinking and drying, outside micro- hollow fibre
Diameter is 70 microns, and internal diameter is 50 microns, and 20 centimetres of length is cut from this continuous fiber, they are nailed together or are interweaved
Together, after discharging organic component and being sintered 2 hours at 950 DEG C, Ceramic Hollow Fiber or Ceramic Hollow Fiber net are obtained, is made pottery
The outer diameter of porcelain doughnut is 60um, internal diameter 44um, porosity 37%.
In conclusion the method for Ceramic Hollow Fiber of the preparation based on nanoscale composition granule, by with hydroxyl carboxylic
Acid conversion nanosize metal oxide, carbide, nitride or sulfide powder, at least one solvent and acrylate and pottery
Porcelain block mixing manufacture ceramic block and/or methacrylate are as polymer adhesive, metal oxide, carbide, nitride
Or the partial size of sulfide powder is 1-50nm, the solid content of ceramic masses is greater than 30%；Be added into ceramic block it is carbon-based, it is organic
Or inorganic component is as expendable material, in an amount of from 5-20wt%；Ceramic block is squeezed or is spun to doughnut blank；By making
With radial starter polymeric acrylate and/or methacrylate adhesives；It is sintered blank, forms outer diameter 100um, aperture
Fiber between 0.5-100nm, the doughnut produced in this way should be porous respectively according to application field or burn
Form close to theoretical density.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of method for preparing the Ceramic Hollow Fiber based on nanoscale composition granule, including hydroxycarboxylic acid, nanoscale powder
End, solvent, polymer adhesive, device for spinning and radial starter.
2. a kind of method for preparing the Ceramic Hollow Fiber based on nanoscale composition granule according to claim 1,
Be characterized in that: the nanometer grade powder includes unstable zirconium oxide, titanium oxide, silicon carbide and the carbonization of aluminium oxide, zirconium oxide, yttrium
Tungsten/or silicon nitride.
3. a kind of method for preparing the Ceramic Hollow Fiber based on nanoscale composition granule according to claim 1,
Be characterized in that: the hydroxycarboxylic acid is selected from trioxa capric acid and dioctyl enanthic acid.
4. a kind of method for preparing the Ceramic Hollow Fiber based on nanoscale composition granule according to claim 1,
Be characterized in that: the solvent is water, ethylene glycol, propylene glycol, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether and ethylene glycol and two
The mixture of ethylene glycol monobutyl ether.
5. a kind of method for preparing the Ceramic Hollow Fiber based on nanoscale composition granule according to claim 1,
Be characterized in that: the polymer adhesive is cellulose, methylcellulose, ethyl cellulose, polyvinyl alcohol, carboxymethyl cellulose
Sodium and polyacrylate/or polymethacrylates.
S1, preferably batch of material contain nano-scale particle, regardless of whether handling Si, Al, B, Zn, Zr, Cd, Ti, Ce, Sn, the oxidation of In
Object, oxide hydrate, chalcogenide, nitride or carbide, La, Fe, Cu, Ta, Nb, V, Mo or W are particularly preferably aoxidized
Object, preferred nano grade inorganic solid granulates are aluminium oxide, zirconium oxide, titanium oxide, silicon carbide, tungsten carbide and silicon nitride, this batch
The average grain diameter of inorganic particle contained in material is usually 1 to 300nm or 1 to 100nm, preferably 5 to 50nm, particularly preferably extremely
20nm, primary granule can also exist with agglomerated form, but preferably not agglomeration or substantially not agglomeration.
The selection and configuration of S2, polymer adhesive are especially commonly used in that squeezed out using any thermoplastic polymer
A bit, such as polyethylene, bialkyl ortho phthalate (repefral, diethyl phthalate, phthalic acid two
Propyl ester, dibutyl phthalate), polypropylene and poly- 1- butane, poly- methyl (methyl) acrylate, polyacrylonitrile, polyphenyl second
Alkene and polyvinyl alcohol, polyamide, polyester, poly- acetic acid esters, polycarbonate, linear polyester and corresponding copolymer, such as ethylene-second
Vinyl acetate (EVA) copolymer and biopolymer such as cellulose and ancient Chinese name for Venus etc., wherein polyacrylate, polymethyl
Acid esters, cellulose and keel glue be it is preferred, the mixed of thermoplastic polymer or two or more thermoplastic polymers can be used
Object is closed, after shaping by using radical initiator, to radiate for example, by UV using acrylate and methacrylate
Or be crosslinked by hot method, form required polymer.
S3, initial powder is mixed with organic bond, wherein at least one polymer adhesive and at least one hydroxycarboxylic acid
With at least one solvent.
S4, in conventional mixing and kneader device, nanometer grade powder and polymer, oxa- carboxylic acid and solvent or solvent mixture
Mixing carries out the mixed of enough time using kneader, double screw extruder, heavy roll squeezer, three roller looms or mortar grinder
It closes and mediates, obtain uniform mixture.
S5, sintering blank.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1211966A (en) * | 1996-01-21 | 1999-03-24 | K·瑞纳贝克 | Hollow microfiber of ceramic material, process for its manufacture and its use |
| CN1503767A (en) * | 2001-04-21 | 2004-06-09 | ITN-��ŵ��ʥ����˾ | Functional ceramiclayers based on a support layer produced with crystalline nanoparticles |
| US20060154057A1 (en) * | 2002-08-30 | 2006-07-13 | Ralph Nonninger | Ceramic hollow fibers made from nanomscale powder particles |
| CN101172856A (en) * | 2007-11-27 | 2008-05-07 | 中国建筑材料科学研究总院 | Method for producing zirconium oxide fibre |
| CN104785123A (en) * | 2015-03-13 | 2015-07-22 | 海门市森达装饰材料有限公司 | Hollow fiber ceramic membrane production method |
-
2019
- 2019-02-15 CN CN201910115693.1A patent/CN109721339A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1211966A (en) * | 1996-01-21 | 1999-03-24 | K·瑞纳贝克 | Hollow microfiber of ceramic material, process for its manufacture and its use |
| CN1503767A (en) * | 2001-04-21 | 2004-06-09 | ITN-��ŵ��ʥ����˾ | Functional ceramiclayers based on a support layer produced with crystalline nanoparticles |
| US20060154057A1 (en) * | 2002-08-30 | 2006-07-13 | Ralph Nonninger | Ceramic hollow fibers made from nanomscale powder particles |
| CN101172856A (en) * | 2007-11-27 | 2008-05-07 | 中国建筑材料科学研究总院 | Method for producing zirconium oxide fibre |
| CN104785123A (en) * | 2015-03-13 | 2015-07-22 | 海门市森达装饰材料有限公司 | Hollow fiber ceramic membrane production method |
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