CN104909820B - Porous ceramics that duct uniformly penetrates and its production and use - Google Patents
Porous ceramics that duct uniformly penetrates and its production and use Download PDFInfo
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Abstract
Porous ceramics that duct uniformly penetrates and its production and use.Penetrated the invention discloses a kind of duct three-dimensional, porosity is uniform, the adjustable porous ceramics preparation method of hole dimension linearity.The raw material that the present invention uses is uniform low activity compact spheroidal particle, and the contact portion of spheric granules forms sintering neck offer ceramics strength by sintering, and the accumulation gap of spheric granules forms 3 D pore canal.Exemplary manufacturing process is：By a certain amount of organic monomer, MBAM, (NH4)2S2O4, TEMED mixing, it is configured to premixed liquid；Premixed liquid is poured into low activity compact spheroidal particle, controls premixed liquid addition, and the tightly packed of spheric granules is realized with certain method；The particle stack that will have been accumulated, it is placed under certain temperature and solidifies；Then the base substrate consolidated is dried and sintered, and obtains the porous ceramics.Porous ceramics prepared by the present invention has good separative efficiency and flux, while can be widely used in the fields such as filtering high-temperature flue gas, melt filtration in oil water mixture separation.
Description
Technical field
The present invention relates to porous ceramics field, more particularly to uniform pore diameter is controllable, the porous ceramics system of the three-dimensional insertion in duct
It is standby.
Background technology
Porous ceramic film material has penetrated into various fields, environmental protection, energy-conservation, chemical industry, oil, smelting, food, pharmacy, life
Multiple scientific domains such as thing medical science all be unable to do without porous ceramic film material, especially filtering, sound-absorbing, electrode material, catalysis, it is heat-insulated,
Biomaterial etc. plays the role of irreplaceable.
The Pore Characteristics of porous ceramic film material determine its performance, and the uniformity and connectivity in duct are to porous ceramics performance
With material impact.Journal of membrane science magazines in 2006 are in volume 285, the first phase, 173-181 pages
In describe the porous ceramic film that 6.3 μm of average pore size is prepared with the irregular fly ash grain of form, find ceramic membrane aperture
Inequality, obvious duct defect be present, pore-size distribution is wider, is difficult to avoid filtering out for fine particle during being separated by filtration.
Good duct connectivity not only contributes to improve flux, and can be still the flowing of fluid when cell channels block
More path is provided, so as to maintain good flux.In addition, uniformly insertion duct is for reducing stress concentration, dimension
The mechanical stability for holding filter has great advantage.At present, the preparation technology comparatively perfect of porous ceramics, air hole structure, divide
Cloth, the regulation and control of size are relatively ripe, but are difficult still to obtain the porous ceramics that substantially uniformity penetrates in three dimension scale.
Powder sintering is a kind of traditional pore-creating technique, and it is sintered after ceramic powder is accumulated, particle contact
Position is sintered together by mass transfer, there is provided ceramics strength, and the reservation in situ after sintering of particle packing gap, turns into porous pottery
Porcelain duct.The technology has the characteristics of simple, direct, without additionally aiding in pore-creating.
But conventional powder improves diffusion mass transfer when preparing porous ceramics by powder sintering often through heating
Speed, neck sintering is formed, this can inevitably result in the melting of particle surface and sintering, cause the contraction and closing in duct.
Because the particle that conventional ball mill or wet method obtain, its surface and inside have numerous defects, specific surface area also tends to
It is larger, there is higher sintering activity.These active crystal faces can promote particle surface to melt in sintering process, reduce diffusion
Mass transfer is leading effective temperature section, accelerates mass transfer mode and is changed into the liquid flowing biography unfavorable to pore structure from diffusion mass transfer
Matter, cause to sinter the generation contradiction between the reservation in situ of neck intensity and duct.Fundamentally say, the source of contradiction is exactly conventional powder
There is no obvious temperature difference between diffusion into the surface mass transfer and melting mass transfer in sintering, it is impossible to only rely on the side for improving sintering temperature
Formula obtains high-strength sintered neck without the hole between influenceing particle.In addition, agglomerated particle present in powder, in sintering process
In can also collapse and drastically shrink, have a strong impact on the formation in duct.
In order to overcome these problems present in powder sintering, people take many methods, for example, microwave sintering,
Hot pressed sintering, discharge plasma sintering and electric spark sintering etc., these methods are provided to shorten sintering time and reinforcing
The diffusion mass transfer of intergranular so that hole has little time to shrink and retained；Sintering temperature can be also reduced to a certain extent simultaneously,
Melt surface degree is reduced, prevents intergranular reunion activated sintering.
In addition, by introducing nanocrystal, neck sintering activity is improved, promotes mass transfer, sintering temperature is reduced, can also carry
While height sintering neck intensity, the contraction of hole is reduced.The chemical reaction between feed particles can also be used, promotes neck to strengthen
Sintering, reduces the contraction of hole.Generation low melting point oxide can also be aoxidized in particle surface, particle is carried out using the oxide
Between mass transfer sinter obtain intensity raising sintered neck.
In a word, the contraction of the inhomogeneities in powder sintering accumulation early stage hole and later stage sintering process hole, makes porous pottery
Porcelain often has wide in range pore-size distribution, containing part lipostomous, half-via, connectivity deficiency, limits porous ceramics and is dividing
From the application in field.
The content of the invention
(1) goal of the invention
The defects of preparing porous ceramics for existing powder sintering, the technical problem that this patent solves are lived using sintering
The relatively low compact spheroidal particle of property, by tightly packed pore-creating between powder particle, utilizes tightly packed interparticle contact part shape
The surface fine and close into neck sintering and low activity is difficult that the characteristics of melt surface sinters, after high temperature sintering, granulation mass occurs
Product neck forms sintering, there is provided ceramics strength, accumulation gap remain to form uniform duct.The side provided using this patent
Method, sintering is accumulated using the active relatively low compact spheroidal particle of uniform particle diameter, can be formed with the more of uniformly insertion duct
Hole ceramics.The duct has the characteristic of uniform, three-dimensional insertion, and porous ceramics has higher intensity.
(2) technical scheme
The powder material that the present invention uses, there is the characteristics of good sphericity, uniform particle sizes, densification, relatively low sintering activity, be
Prepared by heat plasma technology.
By certain accumulation mode, good sphericity, the particle of uniform particle diameter can form tightly packed, accumulation gap energy
Enough form the hole of uniform, the three-dimensional insertion in duct.
From casting molding technique, the original advantage that the technique has in spheric granules banking process is mainly considered：
Particle be initially formed it is tightly packed, then organic reactant mass-energy particulate interspaces polymerize form network structure, make tightly packed
Spheric granules form bonding, the process of bonding will not cause any impact to the arrangement of particle.And in organic substance burn off mistake
Cheng Zhong, catabolite can be excluded thoroughly from the accumulation gap of particle, and particle stack structure is constant.
In sintering process, fine and close particle can avoid particle that itself occurs collapsing, and block duct.Low frit activity energy
Make particle during mass transfer sinters and to form sintered neck, effectively avoid melt surface from triggering particle re-arrangement, stomata contraction etc..It is logical
Cross optimization sintering temperature, it is possible to achieve particle neck effectively sinters, and the rearrangement between melting and particle does not occur for particle surface, obtains
Obtain high intensity, the porous ceramics of duct insertion.
The preparation of the porous ceramics is divided into three committed steps：
A spheric granules is accumulated, and obtains the particle stack of uniform, the three-dimensional insertion of accumulation hole.
Above-mentioned particle stack is carried out in-situ consolidation, form green compact by B using the solidifying system of note.
Green sintering is formed sintered neck by C between particle, hole is in situ to be retained and forms duct.
The uniformly insertion duct is enclosed heap by spherical wall and formed, pattern rule.
It is worth noting that, the granularity by controlling spheric granules, linearly can regulate and control to accumulate the size in duct, finally
It is capable of the pore size of linear regulation porous ceramics.
The invention provides a kind of preparation method in smooth duct, that is, pass through smooth, spherical particle packing boring technique.Separately
Outside, the roughness of channel surfaces can also be regulated and controled by controlling the roughness of spherical particle surface.
The present invention also provides the step of note solidification forming and technological parameter.By the compact spheroidal particle of certain content, organosilicon prepolymer
Mixed liquid (organic monomer, crosslinking agent, water), catalyst, initiator are well mixed so that spheric granules heap in particular manner
Product, then by regulating and controlling temperature initiated polymerization, high intensity green compact are obtained after fully drying, are finally sintered, obtain mesh
Mark porous ceramics.
In some embodiments, the organic monomer is acrylamide, and crosslinking agent is N,N-DMAA
(MBAM), catalyst is tetramethylethylenediamine (TEMED), and initiator is ammonium persulfate, and the concentration of premixed liquid is with acrylamide
Concentration marks.
In some embodiments, the premixed liquid concentration is 2-20wt.%.
In some embodiments, MBAM and organic monomer mass ratio are 1:30-1:10.
In some embodiments, (NH4)2S2O4Occupy the 3-10% of machine monomer mass fraction.
In some embodiments, (NH4)2S2O4Mass ratio with TEMED is 1:1-1:6.
In some embodiments, the reaction temperature of the polymerisation is 30-80 DEG C, reaction time 10-90min.
In some embodiments, the accumulation mode of spheric granules is accumulated for slurry, or natural subsidence accumulation, or centrifugation is heavy
Drop accumulation, or tapped bulk again after natural subsidence.
The present inventor, by a series of exploration, by the influence factor for regulating and controlling each link of casting molding technique
And the accumulation mode of uniform-spherical particle, obtain the porous ceramic film material that duct uniformly penetrates.By being from average grain diameter
30-90 μm of spheric granules, ceramic body average pore size are linearly distributed between 8-20 μm, and percent opening is between 30-45%, pottery
Porcelain body intensity can reach 30MPa, and the material is in wastewater treatment, dedusting, gas distribution, support body material, filtering high-temperature flue gas
Or melt filtration etc. has good application prospect.
(3) technique effect
The porous ceramics that the present invention obtains have duct uniformly, three-dimensional insertion, aperture can linearly reconcile intensity it is high the characteristics of,
Compared with porous ceramics prepared by existing powder sintering, not only duct is uniform, whole duct insertions, and porous ceramics is strong
Degree is high.No matter the porous ceramics that gas or liquid are prepared by the present invention, flux are obviously improved.Will be of the present invention porous
Ceramic applications obtain good oil-water separation, and separating rate is fast in water-oil separating.It is using the thickness of preparation
5mm, the tubular porous ceramic filter that aperture is 8 μm progress peanut oil/water separable performance can be tested：Prepared at 60 DEG C by stirring
1vol.% peanut oil solution, the oil water mixture is relatively uniform, and oil is dispersed in water in the form of micro emulsion oil droplet, initially
TOC values are 843mg/L.Porous ceramic pipe is subjected to water-oil separating under 30KPa, is as a result shown as：Water-oil separating efficiency reaches
More than 99%；Initial flux reaches 105L/(m2H), flux stabilized after 40min, and it is smaller to decline degree, maintains 4.0 ×
104L/(m2h)；By 10 filtering-backwash cycles, filter flux still maintains initial level.It these results suggest that, this hair
Bright prepared hole is uniform, the filter without hole defect, has very high filter efficiency；Its higher flux is from three-dimensional
The connectivity in duct, flow of fluid is unobstructed, and drag losses is small；Insertion duct is the multi-path selection that flow of fluid is brought, and is made
There is porous ceramics good flux to maintain ability；Smooth duct characteristic makes dirty substance be not easy to adhere to, fouling product during backwash
Readily wash off, bring good cycle applications ability.
Brief description of the drawings
Accompanying drawing 1 is the flow chart that the present invention prepares porous ceramics.
Accompanying drawing 2 is the porous ceramics cross-section photographs that uniform pore diameter, three-dimensional prepared by the present invention penetrate.
Embodiment
The preparation process of the present invention is described further with reference to accompanying drawing 1.
Uniform pore diameter, the preparation flow figure of the three-dimensional porous ceramics penetrated are as shown in Figure 1：
(1) compact spheroidal particle of low frit activity refers to the specific surface area of particle close to the spheric granules of theoretical value, this
A little particles can be obtained by melting, melted and obtained in particular by hot plasma nodularization.
(2) configuration of premixed liquid：According to organic monomer 2-20wt.%, MBAM is 1 with organic monomer mass ratio:30-1:
10, configure premixed liquid.
(3) premixed liquid is poured into spheric granules, adds catalyst, initiator, be well mixed, and it is real with specific method
Now spheric granules is tightly packed.Wherein (NH4)2S2O4Occupy the 3-10% of machine monomer mass fraction, (NH4)2S2O4With TEMED
The mass ratio of polyalcohol is 1:1-1:6.
(4) by the good particle of above-mentioned accumulation, progress polymerisation solidification, reaction time 10- at 30-80 DEG C are placed in
90min。
(5) base substrate being cured is placed at 50-70 DEG C and continues to solidify, hardening time 5-15h, realize that base substrate is done
It is dry.
(6) different spheric granules is directed to, dry base substrate sinters 2-5h at 1200-1700 DEG C, obtains described more
Hole ceramics.The section of porous ceramics is as shown in Figure 2.
Embodiment 1
According to organic monomer 2wt.%, MBAM is 1 with organic monomer mass ratio:30, (NH4)2S2O4Occupy machine monomer mass
The 3% of fraction, (NH4)2S2O4Mass ratio with TEMED polyalcohols is 1:1 ratio, configure mixed liquor.Mixed liquor is poured into grain
In the spherical silica particle in 30 μm of footpath, premixed liquid addition is controlled, uniform slurry is configured to, is placed at 80 DEG C, polymerization is anti-
It is 10min between seasonable.After body drying, 1200 DEG C of sintering 2h, 8 μm of average pore size, intensity 25MPa porous ceramics are obtained.
Embodiment 2
According to organic monomer 6wt.%, MBAM is 1 with organic monomer mass ratio:20, (NH4)2S2O4Occupy machine monomer mass
The 5% of fraction, (NH4)2S2O4Mass ratio with TEMED polyalcohols is 1:2 ratio, configure mixed liquor.Mixed liquor is poured into grain
Footpath is in 50 μm of spherical silica particle, controls premixed liquid addition, is configured to uniform slurry, is placed at 70 DEG C, is polymerize
Reaction time is 20min.After body drying, 1200 DEG C of sintering 2h, 15 μm of average pore size, intensity 15MPa porous ceramics are obtained.
Embodiment 3
According to organic monomer 10wt.%, MBAM is 1 with organic monomer mass ratio:20, (NH4)2S2O4Account for organic monomer matter
Measure the 7% of fraction, (NH4)2S2O4Mass ratio with TEMED polyalcohols is 1:3 ratio, configure mixed liquor.Mixed liquor is poured into
Particle diameter is in 50 μm of spherical silica particle, adds excessive premixed liquid, and stirring is stood, by the particle in liquid phase after natural subsidence
Jolt ramming, it is placed at 50 DEG C, polymerization reaction time 40min.After body drying, 1200 DEG C of sintering 2h, 10 μm of average pore size is obtained,
Intensity 27MPa porous ceramics.
Embodiment 4
According to organic monomer 15wt.%, MBAM is 1 with organic monomer mass ratio:15, (NH4)2S2O4Account for organic monomer matter
Measure the 8% of fraction, (NH4)2S2O4Mass ratio with TEMED polyalcohols is 1:4 ratio, configure mixed liquor.Mixed liquor is poured into
Particle diameter is in 50 μm of spherical silica particle, adds excessive premixed liquid, and stirring is stood, by the particle in liquid phase after natural subsidence
Jolt ramming, it is placed at 50 DEG C, polymerization reaction time 40min.After body drying, 1300 DEG C of sintering 2h, 7 μm of average pore size is obtained,
Intensity 35MPa porous ceramics.
Embodiment 5
According to organic monomer 20wt.%, MBAM is 1 with organic monomer mass ratio:10, (NH4)2S2O4Account for organic monomer matter
Measure the 10% of fraction, (NH4)2S2O4Mass ratio with TEMED polyalcohols is 1:6 ratio, configure mixed liquor.Mixed liquor is fallen
Enter in the spherical silica particle that particle diameter is 50 μm, add excessive premixed liquid, stirring is stood, by liquid phase after natural subsidence
Grain jolt ramming, is placed at 50 DEG C, polymerization reaction time 40min.After body drying, 1300 DEG C of sintering 5h, the μ of average pore size 5 is obtained
M, intensity 40MPa porous ceramics.
Embodiment 6
According to organic monomer 2wt.%, MBAM is 1 with organic monomer mass ratio:30, (NH4)2S2O4Occupy machine monomer mass
The 3% of fraction, (NH4)2S2O4Mass ratio with TEMED polyalcohols is 1:1 ratio, configure mixed liquor.Mixed liquor is poured into grain
In the Spherical alumina particles that 30 μm of footpath, premixed liquid addition is controlled, uniform slurry is configured to, is placed at 80 DEG C, polymerization is anti-
It is 10min between seasonable.After body drying, 1700 DEG C of sintering 2h, 8 μm of average pore size, intensity 28MPa porous ceramics are obtained.
Embodiment 7
According to organic monomer 2wt.%, MBAM is 1 with organic monomer mass ratio:30, (NH4)2S2O4Occupy machine monomer mass
The 3% of fraction, (NH4)2S2O4Mass ratio with TEMED polyalcohols is 1:1 ratio, configure mixed liquor.Mixed liquor is poured into grain
In the spherical mullite particle in 30 μm of footpath, premixed liquid addition is controlled, uniform slurry is configured to, is placed at 80 DEG C, polymerization is anti-
It is 10min between seasonable.After body drying, 1700 DEG C of sintering 2h, 8 μm of average pore size, intensity 30MPa porous ceramics are obtained.
Embodiment 8
According to organic monomer 10wt.%, MBAM is 1 with organic monomer mass ratio:12, (NH4)2S2O4Account for organic monomer matter
Measure the 8% of fraction, (NH4)2S2O4Mass ratio with TEMED polyalcohols is 1:3 ratio, configure mixed liquor.Mixed liquor is poured into
Particle diameter is in 30 μm of magnesia spheric granules, adds excessive premixed liquid, and stirring is stood, by the particle in liquid phase after natural subsidence
Jolt ramming, it is placed at 50 DEG C, polymerization reaction time 40min.After body drying, 1800 DEG C of sintering 2h, 8 μm of average pore size is obtained,
Intensity 50MPa porous ceramics.
Embodiment 9
According to organic monomer 20wt.%, MBAM is 1 with organic monomer mass ratio:15, (NH4)2S2O4Account for organic monomer matter
Measure the 15% of fraction, (NH4)2S2O4Mass ratio with TEMED polyalcohols is 1:6 ratio, configure mixed liquor.Mixed liquor is fallen
Enter particle diameter for 25 μm, composition is magnesium aluminate spinel (MgAl2O4) spheric granules in, add excessive premixed liquid, stirring is stood, from
So the particle jolt ramming in liquid phase is placed at 50 DEG C, polymerization reaction time 40min after sedimentation.After body drying, 1700 DEG C of burnings
5h is tied, obtains 5 μm of average pore size, intensity 40MPa porous ceramics.
Embodiment 10
According to organic monomer 7wt.%, MBAM is 1 with organic monomer mass ratio:8, (NH4)2S2O4Occupy machine monomer mass
The 10% of fraction, (NH4)2S2O4Mass ratio with TEMED polyalcohols is 1:6 ratio, configure mixed liquor.Mixed liquor is poured into
Particle diameter is in 20 μm of spherical SiC particulate, adds excessive premixed liquid, and stirring is stood, and the particle in liquid phase shakes after natural subsidence
It is real, it is placed at 50 DEG C, polymerization reaction time 40min.After body drying, 1700 DEG C of sintering 5h, 4 μm of average pore size is obtained, by force
Spend 45MPa porous ceramics.
Claims (3)
1. the preparation method for the porous ceramics that a kind of duct uniformly penetrates, it is characterised in that comprise the following steps：
(1) organic premixed liquid is prepared：Organic monomer, crosslinking agent and water are formed into organic premixed liquid；
(2) particle packing：Organic premixed liquid is added in low frit active dense spheric granules prepared by heat plasma technology,
It is well mixed after adding catalyst and initiator, and the tightly packed of spheric granules is realized with specific method, particle packing
Method includes jolt ramming after slurry accumulation, natural subsidence, centrifugal sedimentation, natural subsidence；
(3) solidification forming is noted：Regulating and controlling temperature initiated polymerization, high intensity green compact are obtained after fully drying；Polymerisation
Reaction temperature is 30-80 DEG C, reaction time 10-90min；50-70 DEG C of drying temperature, drying time 5-15h；
(4) green sintering：By green sintering, particle forms porous ceramic skeleton, and sintered neck is formed between particle, and hole is in situ to be protected
Stay to form duct；Sintering temperature is 1200-1700 DEG C, sintering time 2-5h；
The percent opening of the porous ceramics is between 30-45%, and between 8-20 μm, the porous ceramics intensity is average pore size
15-40MPa。
2. according to the method for claim 1, it is characterised in that organic monomer described in step (1) is acrylamide, crosslinking
Agent is N,N-DMAA, and catalyst is tetramethylethylenediamine described in step (2), and initiator is ammonium persulfate.
3. according to the method for claim 2, it is characterised in that the concentration of organic premixed liquid is with the concentration of acrylamide
2-20wt% is labeled as, N,N-DMAA is 1 with organic monomer mass ratio:30-1:10, ammonium persulfate occupies machine list
The mass ratio of the 3-10% of weight fraction, ammonium persulfate and tetramethylethylenediamine is 1:1-1:6.
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| CN106747346B (en) * | 2016-11-15 | 2019-06-21 | 中国科学院过程工程研究所 | A kind of porous ceramic film and preparation method |
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| CN111099913B (en) * | 2020-01-03 | 2022-01-14 | 内蒙古工业大学 | Raw material for preparing porous ceramic material and preparation method of porous ceramic material |
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| CN113387694B (en) * | 2021-06-24 | 2023-03-21 | 重庆奥福精细陶瓷有限公司 | Particle filter and preparation method thereof |
| CN113786689A (en) * | 2021-09-22 | 2021-12-14 | 重庆奥福精细陶瓷有限公司 | Narrow micropore distribution cordierite honeycomb ceramic filter and preparation method and application thereof |
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