CN101712561A - Method for preparing SiC porous ceramic by splicing clay - Google Patents
Method for preparing SiC porous ceramic by splicing clay Download PDFInfo
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- CN101712561A CN101712561A CN200910193875A CN200910193875A CN101712561A CN 101712561 A CN101712561 A CN 101712561A CN 200910193875 A CN200910193875 A CN 200910193875A CN 200910193875 A CN200910193875 A CN 200910193875A CN 101712561 A CN101712561 A CN 101712561A
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Abstract
The invention discloses a method for preparing SiC porous ceramic by splicing clay, and is characterized by comprising the following processes of selection and proportioning of raw materials, mixing, pelleting, isopressing and sintering; the raw materials are proportioned as follows: SiC accounts for 70-80 wt%, ledikite clay accounts for 7-20 wt% and graphite accounts for 0-15wt %; the grain diameter of the SiC particle is 200-450 mu m, and the grain diameter of the graphite is 50-250 mu m; the obtained pelleting particle material forms a green body on a mould; and the green body is pressed for forming in an isopressing press of 100-400 MPa, and finally sintering is carried out. Compared with the prior art, the manufactured porous ceramic of invention has the advantages of high porosity, evenly pore distribution and pore size, large strength, non-deformation, low-degree degradation of performance, long service life and low manufacturing cost.
Description
Technical field:
The present invention relates to a kind of making method of filtering with porous ceramics.
Background technology:
In the cleaning coal combustion technology, how handling high-temperature dust gas is a difficult problem, the ideal method is a dust removal by filtration, its key is the selection of filtering material, China mainly adopts glass fibre to do filtering material, but it can only adopt the method that refilters after the dilution air cooling processing through can't stand high temperature more than 400 ℃ to temperature flue gas on it, has reduced filtration efficiency.In order to address the above problem, people have invented the rigidity porous ceramics again.High-temperature dust removal adopts the rigidity porous ceramics, and supporter also requires at high temperature have enough physical strengths except that requiring to have certain pore size, distribution and the porosity, can stand the pressure that blowback is cleaned, and is not yielding under use temperature.The refractoriness of skeleton material own wants high for this reason, and liquid phase can not occur under use temperature.It is that thermal shock resistance is good that another one requires, and the cold cycling that is able to take blowback cold air is impacted, and guarantees work-ing life, and it is necessary adopting the low thermal coefficient of expansion material for this reason, and can not change through the thermal shock material-structure, and creep resistance is good.
A kind of Hot Gas Cleaning Using For Refractory Ceramics Filter Element of patent 200410023972 inventions, ceramic fiber composite membrane by ceramic supporting body and its outside surface is formed, the conventional hot pouring moulding process of moulding, it is aggregate that supporter adopts trichroite, high temperature adhesives adopts potassium felspar sand, strong flux raw material such as triphane and talcum, and content is at 10-30%, firing temperature is 1230-1260 ℃, the aperture is at 100-150um, void content 35-40%, bending strength 15-25MPa, 950-20 ℃ of circulation impact of high high-temp stability index do not split for 10 times, be subjected to self physical properties of ceramic fiber composite membrane to determine that the ceramic fiber composite membrane is impaired easily, and the performance of impaired back product is just seriously influenced; A kind of in-situ reaction of patent 200510029152 inventions prepares the method for the carborundum porous ceramics of mullite bonded, and two-sided pressurization drawing method is adopted in moulding, is that pore-forming material, yttrium oxide are sintering aid with graphite, and oxidation generates SiO under the SiC high temperature
2, again by the SiO that generates
2Directly and Al
2O
3The particle in-situ reaction generates mullite, is prepared into the carborundum porous ceramics of mullite bonded, and open porosity is 20-70%, and maximum bending strength can reach 27.5MPa, thermal expansivity 6-9*10
-6K
-1Quenching test: porous ceramics entered suddenly under 1200 ℃ high temperature 20 ℃ the cold water, the intensity of porous ceramics is reduced to 4.09MPa from 9.84MPa, and technological merit is to add Y
2O
3Reduce mullite and generate 100 ℃ of temperature, higher porosity and intensity, lower thermal expansivity, good heat shock resistance and porosity and pore size are controlled, but thermal shock resistance is poor, and the cold cycling that is not able to take blowback cold air is impacted, and work-ing life is bad; Patent 200610119233 adopts preparing silicon carbide porous ceramic using gelatin wrapping-freeze drying process, own aluminum isopropylate and SiC generate the silicon carbide of mullite bonded for the main raw material reaction in, mechanical stirring is prepared into disperses uniform slurry, adopt casting, vacuum outgas, the quick freezing moulding, low pressure environment will be iced distillation and form high porosity, the porous body that the aperture aligns, open porosity is between 40-90%, aperture size is 1-500um, ultimate compression strength is between 0.09-12.3MPa, the invention advantage is to prepare high porosity, the microvoid structure of hole orientation, have the good characteristics of mullite bonded silicon carbide ceramics inherent high-temperature behavior concurrently, still, ultimate compression strength is not enough; Patent 200510003016 has been invented a kind of preparation method of recrystallized SIC high temperature gas filter element; pile up pore-forming and add the mode pore-forming that auxiliary pore-forming material pore-forming combines with special bomodal size distribution; isostatic pressing; pressure 20-200MPa; Ar-sintering; firing temperature 2000-2300 ℃; pressure 0.1-0.3MPa; SiC material purity 98-99% needs through purification processes mean pore size 30-100um; porosity 20-40%; bending strength 15-35MPa, the invention advantage be SiC content up to 98.5%, do not contain wedding agent; physical strength and structural stability are fabulous; alleviated the degeneration of material performance under Working environment, and recrystallization SiC sintering do not shrink, can obtain accurate product size and be easy to control the aperture and the pore size distribution range of perforate; but owing to need higher forming temperature; therefore, technology controlling and process complexity, manufacturing cost height.
Above-mentioned several technology, though, on some technical indicators, can reach requirement,, some defectives are always arranged, the product that manufacturing is come out can not satisfy service requirements fully.
Summary of the invention:
Goal of the invention of the present invention be to provide the porous ceramics that a kind of manufacturing comes out porosity height, pore size, be evenly distributed, intensity is big, indeformable, the performance degradation degree is low, the method for the preparing SiC porous ceramic by splicing clay of long service life, low cost of manufacture.
The present invention is achieved in that and comprises material choice proportioning, batch mixing granulation, isostatic pressing and firing process, wherein,
In the material choice proportioning:
(a) account for 70-80wt% by SiC, (illite clay is a kind of rich potassium, high alumina layer silicate mineral to illite clay, illite clay is the major name of this mineral) account for 7-20wt%, graphite accounts for 0-15wt% and prepares burden, the SiC particle grain size is between 200-450um, and the particle diameter of graphite is between 50-250um;
(b) add the PVAC polyvinylalcohol that accounts for batching total mass 0.1-0.5wt% in the admixtion of (a) step gained and do the moulding caking agent, adding batching gross weight 1-5 water doubly is dispersion medium, the ball grinder batch mixing of packing into;
(c) step (b) gained slurry is carried out mist projection granulating, granulation material moisture content is below 2%, and the particulate material that is obtained is configured as base substrate on mould, waiting in the static pressure press of 100-400MPa base substrate is pressed then;
(d) body drying that compression moulding is good carries out sintering then under 1300-1500 ℃ air atmosphere.
Sintering mechanism of the present invention is liquid phase sintering, utilizes illitic flux characteristic, at high temperature forms liquid phase, and the SiC porous ceramics is realized sintering, and graphite is pore-forming material.Because adopt illite to cooperate SiC to carry out sintering, like this, the splicing clay carborundum porous ceramics that utilizes the present invention to prepare has the following advantages:
(1) by improving sintering temperature, reduces the consumption of high temperature adhesive, can reach the creep-resistant property of material is improved, do not try the strength of materials again and descend a lot, by the remedying of technology, can try intensity and be improved on the contrary;
(2) by the preferably clay material, the content of the quartz particles that reduction can undergo phase transition has been realized the raising of porous ceramics cold-and-heat resistent impact property;
(3) pressure of raising isostatic pressing reduces the influence of particle packing to material porosity and pore size distribution, and pore-forming material by regulating pore-forming material granular size and content, is realized the controllability of porosity and pore size distribution to the single control of porosity and pore size distribution; Contain a certain amount of clay in the base substrate, the dry body strength height;
(4) the product excellent combination property of the present invention's preparation, preparation technology is simple, and cost is low, is easy to large-scale production.
Here, the illite mineral clay needs to remove harmful quartzy coarse particles through washing, and index of plasticity need be greater than 3.5kg/cm, and the K+Na mass percent is greater than 6.5%;
In order to guarantee to mix and make broken material particles to meet the requirements, with the zirconium white ball-milling medium, the rotating speed that ball mill mixing is needs at 10-100 rev/min, and the ball milling time is 0.5-20 hour, and material ball ratio is 1: 1-10;
Spray-dired drying temperature is no more than 80 ℃, needs to carry out between 900-1000 ℃ moderate heat insulation 1-10 hour;
Here, SiC is α-SiC.
The illite clay raw material is removed the harmful quartzy coarse particles that contains through washing process, and the following particle of 1um accounts for more than 75%.
The present invention compared with the prior art, have the porous ceramics that manufacturing comes out porosity height, pore size, be evenly distributed, intensity is big, indeformable, the performance degradation degree is low, long service life, advantage of low manufacturing cost.
Embodiment:
Now in conjunction with the embodiments the present invention is described in further detail:
The present invention is achieved in that and comprises material choice proportioning, batch mixing granulation, isostatic pressing and firing process, wherein,
In the material choice proportioning:
(a) account for 70-80wt% by SiC, illite clay accounts for 7-20wt%, graphite accounts for 0-15wt% and prepares burden, SiC is α-SiC, the SiC particle grain size is between 200-450um, and the particle diameter of graphite is between 50-250um, and the illite mineral clay needs to remove harmful quartzy coarse particles through washing, and index of plasticity needs greater than 3.5kg/cm, and the K+Na mass percent is greater than 6.5%;
(b) in the admixtion of (a) step gained, add the PVAC polyvinylalcohol that accounts for batching total mass 0.1-0.5wt% and do the moulding caking agent, adding batching gross weight 1-5 water doubly is dispersion medium, the ball grinder batch mixing of packing into, with the zirconium white is ball-milling medium, the rotating speed that ball mill mixing is needs at 10-100 rev/min, the ball milling time is 0.5-20 hour, and material ball ratio is 1: 1-10;
(c) step (b) gained slurry is carried out mist projection granulating, spray-dired drying temperature is no more than 80 ℃, need between 900-1000 ℃, to carry out moderate heat insulation 1-10 hour, granulation material moisture content is below 2%, the granular size of granulation is 100-500um, the particulate material that is obtained is configured as base substrate on mould, waiting in the static pressure press of 100-400MPa base substrate is pressed then;
(d) body drying that compression moulding is good carries out sintering then under 1300-1500 ℃ air atmosphere.
The SiC porous ceramic support open-cell porosity that this prepared goes out is 30-60%, and the aperture is 100-200um, bending strength 20-30MPa, and maximum intensity can reach 45MPa, and volume density is at 1.0-2.0g/cm
3Between, thermal expansivity is at 5-8*10
-6K
-1Between, thermal shock resistance is good, and porous ceramics is put into 20 ℃ cold water suddenly from 1000 ℃ high temperature, circulation according to this, do not ftracture for 30 times, porous ceramics is put into 20 ℃ cold water suddenly from 1000 ℃ high temperature, intensity drops to 16MPa from original 22MPa.In the accelerated weathering test of the element that the present invention makes under the simulation real running environment, material stands the test of 300h, and deterioration does not take place intensity.Boiled in the sulphuric acid soln of 20wt% 1 hour, and carried out the acid corrosion-resistant test, the weightlessness of porous ceramics is 0.1wt%, and sample was boiled in the sodium hydroxide solution of 1wt% 1 hour, and the weightlessness of porous ceramics is 4.2wt%.
Claims (8)
1. the method for a preparing SiC porous ceramic by splicing clay is characterized in that comprising material choice proportioning, batch mixing granulation, isostatic pressing and firing process, wherein,
In the material choice proportioning:
(a) account for 70-80wt% by SiC, illite clay accounts for 7-20wt%, and graphite accounts for 0-15wt% and prepares burden, and the SiC particle grain size is between 200-450um, and the particle diameter of graphite is between 50-250um;
In batch mixing granulation, isostatic pressing:
(b) add the PVAC polyvinylalcohol that accounts for batching total mass 0.1-0.5wt% in the admixtion of (a) step gained and do the moulding caking agent, adding batching gross weight 1-5 water doubly is dispersion medium, the ball grinder batch mixing of packing into;
(c) step (b) gained slurry is carried out mist projection granulating, granulation material moisture content is below 2%, and the particulate material that is obtained is configured as base substrate on mould, waiting in the static pressure press of 100-400MPa base substrate is pressed then;
In firing process:
(d) body drying that compression moulding is good carries out sintering then under 1300-1500 ℃ air atmosphere.
2. the method for preparing SiC porous ceramic by splicing clay according to claim 1 is characterized in that the illite clay index of plasticity needs greater than 3.5kg/cm, and the K+Na mass percent is greater than 6.5%.
3. the method for preparing SiC porous ceramic by splicing clay according to claim 1, the granular size that it is characterized in that granulation in batch mixing granulation, isostatic pressing is 100-500um.
4. according to the method for claim 1 or 2 or 3 described preparing SiC porous ceramic by splicing clay, it is characterized in that with the zirconium white being ball-milling medium, the rotating speed that ball mill mixing is needs at 10-100 rev/min, and the ball milling time is 0.5-20 hour, and material ball ratio is 1: 1-10.
5. according to the method for claim 1 or 2 or 3 described preparing SiC porous ceramic by splicing clay, it is characterized in that spray-dired drying temperature is no more than 80 ℃, need between 900-1000 ℃, to carry out moderate heat insulation 1-10 hour.
6. the method for preparing SiC porous ceramic by splicing clay according to claim 4 is characterized in that spray-dired drying temperature is no more than 80 ℃, needs to carry out between 900-1000 ℃ moderate heat insulation 1-10 hour.
7. the method for preparing SiC porous ceramic by splicing clay according to claim 6 is characterized in that SiC is α-SiC.
8. the method for preparing SiC porous ceramic by splicing clay according to claim 7 is characterized in that illite clay, removes the harmful quartzy coarse particles that contains through washing process, and the following particle of 1um accounts for more than 75%.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320823A (en) * | 2011-06-14 | 2012-01-18 | 淄博工陶耐火材料有限公司 | Artificial jade as well as application and preparation method thereof |
| TWI454441B (en) * | 2011-11-16 | 2014-10-01 | ||
| CN104072142A (en) * | 2014-06-30 | 2014-10-01 | 江苏新光环保工程有限公司 | Preparation method of oxide combined SiC porous ceramic |
| CN104761274A (en) * | 2015-03-26 | 2015-07-08 | 安徽中鼎美达环保科技有限公司 | Silicon carbide porous ceramic and preparation technique thereof |
| CN106422813A (en) * | 2016-09-20 | 2017-02-22 | 芜湖成德龙过滤设备有限公司 | Ceramic filter membrane and preparation method thereof |
| CN115180928A (en) * | 2022-08-09 | 2022-10-14 | 广西碧清源环保投资有限公司 | Porous ceramic blank and preparation method thereof, porous ceramic material and application thereof |
| CN117682865A (en) * | 2024-01-30 | 2024-03-12 | 山东奥福环保科技股份有限公司 | Silicon carbide honeycomb ceramic and preparation method and application thereof |
-
2009
- 2009-11-06 CN CN200910193875A patent/CN101712561A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320823A (en) * | 2011-06-14 | 2012-01-18 | 淄博工陶耐火材料有限公司 | Artificial jade as well as application and preparation method thereof |
| CN102320823B (en) * | 2011-06-14 | 2013-09-25 | 淄博工陶耐火材料有限公司 | Artificial jade as well as application and preparation method thereof |
| TWI454441B (en) * | 2011-11-16 | 2014-10-01 | ||
| CN104072142A (en) * | 2014-06-30 | 2014-10-01 | 江苏新光环保工程有限公司 | Preparation method of oxide combined SiC porous ceramic |
| CN104761274A (en) * | 2015-03-26 | 2015-07-08 | 安徽中鼎美达环保科技有限公司 | Silicon carbide porous ceramic and preparation technique thereof |
| CN104761274B (en) * | 2015-03-26 | 2017-04-26 | 安徽中鼎美达环保科技有限公司 | Silicon carbide porous ceramic and preparation technique thereof |
| CN106422813A (en) * | 2016-09-20 | 2017-02-22 | 芜湖成德龙过滤设备有限公司 | Ceramic filter membrane and preparation method thereof |
| CN115180928A (en) * | 2022-08-09 | 2022-10-14 | 广西碧清源环保投资有限公司 | Porous ceramic blank and preparation method thereof, porous ceramic material and application thereof |
| CN117682865A (en) * | 2024-01-30 | 2024-03-12 | 山东奥福环保科技股份有限公司 | Silicon carbide honeycomb ceramic and preparation method and application thereof |
| CN117682865B (en) * | 2024-01-30 | 2024-04-12 | 山东奥福环保科技股份有限公司 | Silicon carbide honeycomb ceramic and preparation method and application thereof |
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Application publication date: 20100526 |