CN1793040A - Porous ceramic support for high strength inorganic separating film and preparation process thereof - Google Patents
Porous ceramic support for high strength inorganic separating film and preparation process thereof Download PDFInfo
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- CN1793040A CN1793040A CN 200610011191 CN200610011191A CN1793040A CN 1793040 A CN1793040 A CN 1793040A CN 200610011191 CN200610011191 CN 200610011191 CN 200610011191 A CN200610011191 A CN 200610011191A CN 1793040 A CN1793040 A CN 1793040A
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- silicon carbide
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- forming material
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Abstract
The invention relates to a high intension abio-separation film using multi-hole ceramic supporting and the manufacture method. It contains 90-95wt% silicon carbide aggregate, 5-10wt% binding agent and 35-50wt% pore-forming material. Adding binding agent and pore-forming material into beta phase silicon carbide aggregate, grinding, drying, pressing, and molding, sintering at 1280-1360 degree centigrade for 2-6 hours, the material would be gained. It could greatly improve the intension and porosity.
Description
Technical field
The present invention relates to a kind of porous ceramic support for high strength inorganic separating film and preparation method thereof, belong to technical field of ceramic material.
Background technology
Any chemical and metallurgical reaction process always comprise the purifying of raw material and product extraction, concentrate, purification and links such as treatment of wastes produced and cycle applications.Everything all will use separating technology, and often relates to High Temperature High Pressure and other severe environment.As the mould material of a class novel green science and technology, inorganic separating film has a series of characteristics compared with high-polymer membrane: Heat stability is good, and chemical stability is good, the intensity height, Mechanical Builds is stable, can carry out regenerative operations such as the cleaning of soda acid or hot steam, high pressure recoil.For adapting to the purpose of different separating and filterings, on porous ceramic support, will cover the mineral membrane in the different apertures of one deck, but such mineral membrane can't support impressed pressure (＞20MPa) variation separately.Therefore, the surface inorganic film must have supporter to support, and requires the intensity of supporter to want enough height.The coefficient of expansion is low because carborundum porous ceramics has, and heat-shock resistance is strong, characteristics such as favorable mechanical and chemical stability under the high temperature, and its supporter as mineral membrane is widely used in the separating and filtering aspect of support of the catalyst and gas solid separation and molten metal.
According to working conditions, the influence that requires inorganic separating film must be able to bear the variation of air-flow chemical property, change of component and vibrate when spraying into superfine grit, and keep higher efficiency of dust collection, keep high flow capacity and low drop-out nature; Require inorganic separating film can bear mechanical grip power simultaneously, clean vibration force and the thermal stresses that causes because of the air-flow impulse jet.The inorganic separating film that requires to select not only will have stability heat, chemistry, machinery, also should have wearing quality and higher reliability.When having gas phase sulfur, alkali, the corrosion of chlorine element, require inorganic separating film to have very high relative stability.Therefore, under harsh conditions such as High Temperature High Pressure, the intensity of inorganic separating film is had higher requirement, the requirement of this intensity just directly implement to porous ceramic support above.(could add the technology of one section prior art for preparing porous ceramic support, and point out its deficiency).
Summary of the invention
The purpose of this invention is to provide and a kind ofly have high strength, high chemical stability and than open grain, comparatively the inorganic separating film that distributes of uniform pore size is with porous ceramic support material and preparation method thereof.
The high-strength inorganic separation film porous silicon carbide ceramic supporter that the present invention proposes, it is characterized in that: described ceramic supporting body contains the ready-formed carborundum aggregate, binding agent and pore-forming material; The weight percent of described carborundum aggregate is 90-95%, and the weight percent of described binding agent is 5-10%, and the volume percent of described pore-forming material is 35-50%.
In above-mentioned porous silicon carbide ceramic supporter, described carborundum aggregate is the β phase silicon carbide, and particle diameter is 200-300um.
In above-mentioned porous silicon carbide ceramic supporter, described binding agent is that glaze formula is 0.3K
2O (0.7CaO) .0.6Al
2O
3.4.5SiO
2The feldspathic glaze.
In above-mentioned porous silicon carbide ceramic supporter, described pore-forming material is not low 80% a Sodium dodecylbenzene sulfonate of content.
In above-mentioned porous silicon carbide ceramic supporter, described prefabricated carborundum aggregate is by following prepared: pour the SiC powder into ball mill and carry out wet ball mill, behind the thorough mixing, drying, half-dried molded, calcined 2-2.5 hour down at 980-1020 ℃, behind the stove naturally cooling, through the β phase silicon carbide aggregate of pulverizing, sieving and grading is prepared into the variable grain grade.
The preparation method of the porous silicon carbide ceramic supporter that the present invention proposes is characterized in that add binding agent in ready-formed β phase silicon carbide aggregate powder, and add pore-forming material simultaneously, its concrete preparation method comprises following each step:
(1) raw material combination treatment: in ready-formed aggregate β phase silicon carbide powder, add binding agent and pore-forming material, be made into mixed powder, add deionized water and be made into slurry;
(2) with behind the slurry ball milling of step 1 at high temperature drying obtain powder, sieve dry-pressing or cold isostatic compaction;
(3) powder after the moulding is carried out pressureless sintering, sintering temperature is 1280-1360 ℃, and soaking time 2-6 hour, atmosphere was oxidizing atmosphere, gets the porous silicon carbide ceramic supporter with the stove naturally cooling.
Because the present invention forms aggregate and utilizes special process to add technology such as binding agent and pore-forming material by the strict classification of raw material, can greatly improve the intensity and the porosity of porous material.Prepared carborundum porous ceramics has that the coefficient of expansion is low, and heat-shock resistance is strong, excellent over-all properties such as favorable mechanical and chemical stability under the high temperature.Utilize the inorganic separating film of porous silicon carbide material preparation to have in porosity height, hardness height, the wear-resisting and working process characteristics such as chemical transformation do not take place, thereby from material reduced that inorganic separating film in use occurs owing to high temperature wear, hardness descend, fragility causes the probability that lost efficacy greatly, improved work-ing life and the result of use of inorganic separating film.Adopt the pressureless sintering method to improve the production efficiency of porous ceramic support simultaneously in addition, reduced production cost.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
The method of prefabricated carborundum aggregate:
Pour the SiC powder into ball mill and carry out wet ball mill, behind the thorough mixing, drying, half-dried molded, calcined 2 hours down at 980 ℃, behind the stove naturally cooling, be prepared into 200um, the β phase silicon carbide aggregate of 250um and 300um variable grain grade through pulverizing, sieving and grading.
Embodiment one:
With 95 gram particles directly is 300um β phase silicon carbide aggregate, and 5 gram feldspathic glaze and 40Vol.% Sodium dodecylbenzene sulfonate mix, and pour into and carry out ball milling in the 200ml deionized water 24 hours.Slurry 80 ℃ of dryings 24 hours in bipyramid formula revolution vacuum-drying instrument, the granulation of sieving.By the required powder that takes by weighing corresponding weight of reality, be filled in the steel die, under the pressure of 200MPa, add and be pressed into the round tube type supporter.Base substrate is put into the stove corundum crucible, at 1320 ℃, burns till under the condition of insulation 6h, with the stove naturally cooling, prepares a kind of porous silicon carbide ceramic supporter.
Test result is: utilize particle diameter 300um β phase SiC ceramic aggregate, add the 5wt% caking agent, adopt the 40Vol.% Sodium dodecylbenzene sulfonate as pore-forming material, at 1320 ℃, under the firing condition of insulation 6h, the porosity of the SiC porous ceramic support of preparation is 45%, and mean pore size is 60um, and intensity reaches 22MPa.
Embodiment two:
With 95 gram particles directly is 200um β phase silicon carbide aggregate, and 5 gram feldspathic glaze and 35Vol.% Sodium dodecylbenzene sulfonate mix, and pour into and carry out ball milling in the 200ml deionized water 24 hours.Slurry 80 ℃ of dryings 24 hours in bipyramid formula revolution vacuum-drying instrument, the granulation of sieving.By the required powder that takes by weighing corresponding weight of reality, be filled in the steel die, under the pressure of 200MPa, add and be pressed into the round tube type supporter.Base substrate is put into the stove corundum crucible, at 1280 ℃, burns till under the condition of insulation 6h, with the stove naturally cooling, prepares another kind of porous silicon carbide ceramic supporter.
Test result is: utilize particle diameter 200um β phase SiC ceramic aggregate, add the 5wt% caking agent, adopt the 35Vol.% Sodium dodecylbenzene sulfonate as pore-forming material, at 1280 ℃, under the firing condition of insulation 6h, the porosity of the SiC porous ceramic support of preparation is 36%, and mean pore size is 40um, and intensity reaches 23.6MPa.
Embodiment three:
With 90 gram particles directly is 300um β phase silicon carbide aggregate, and 10 gram feldspathic glaze and 35Vol.% Sodium dodecylbenzene sulfonate mix, and pour into and carry out ball milling in the 200ml deionized water 24 hours.Slurry 80 ℃ of dryings 24 hours in bipyramid formula revolution vacuum-drying instrument, the granulation of sieving.By the required powder that takes by weighing corresponding weight of reality, be filled in the steel die, under the pressure of 200MPa, add and be pressed into the round tube type supporter.Base substrate is put into the stove corundum crucible, at 1300 ℃, burns till under the condition of insulation 4h, with the stove naturally cooling, prepares a kind of porous silicon carbide ceramic supporter.
Test result is: utilize particle diameter 300um β phase SiC ceramic aggregate, add the 10wt% caking agent, adopt the 35Vol.% Sodium dodecylbenzene sulfonate as pore-forming material, at 1300 ℃, under the firing condition of insulation 4h, the porosity of the SiC porous ceramic support of preparation is 43%, and mean pore size is 58um, and intensity reaches 24.5MPa.
Embodiment four:
With 90 gram particles directly is 250um β phase silicon carbide aggregate, and 10 gram feldspathic glaze and 40Vol.% Sodium dodecylbenzene sulfonate mix, and pour into and carry out ball milling in the 200ml deionized water 24 hours.Slurry 80 ℃ of dryings 24 hours in bipyramid formula revolution vacuum-drying instrument, the granulation of sieving.By the required powder that takes by weighing corresponding weight of reality, be filled in the steel die, under the pressure of 200MPa, add and be pressed into the round tube type supporter.Base substrate is put into the stove corundum crucible, at 1320 ℃, burns till under the condition of insulation 4h, with the stove naturally cooling, prepares a kind of porous silicon carbide ceramic supporter.
Test result is: utilize particle diameter 250um β phase SiC ceramic aggregate, add the l0wt% caking agent, adopt the 40Vol.% Sodium dodecylbenzene sulfonate as pore-forming material, at 1320 ℃, under the firing condition of insulation 4h, the porosity of the SiC porous ceramic support of preparation is 44.7%, and mean pore size is 57um, and intensity reaches 26.4MPa.Can guarantee under the High Temperature High Pressure working conditions requirement fully to supporter.
Claims (6)
1, high-strength inorganic separation film porous silicon carbide ceramic supporter, it is characterized in that: described ceramic supporting body contains the ready-formed carborundum aggregate, binding agent and pore-forming material; The weight percent of described carborundum aggregate is 90-95%, and the weight percent of described binding agent is 5-10%, and the volume percent of described pore-forming material is 35-50%.
2, according to the described porous silicon carbide ceramic supporter of claim 1, it is characterized in that: described carborundum aggregate is the β phase silicon carbide, and particle diameter is 200-300um.
3, according to the described porous silicon carbide ceramic supporter of claim 1, it is characterized in that: described binding agent is that glaze formula is 0.3K
2O (0.7CaO) .0.6Al
2O
3.4.5SiO
2The feldspathic glaze.
4, according to the described porous silicon carbide ceramic supporter of claim 1, it is characterized in that: described pore-forming material is not low 80% a Sodium dodecylbenzene sulfonate of content.
5, according to the described porous silicon carbide ceramic supporter of claim 1, it is characterized in that: described prefabricated carborundum aggregate is by following prepared: pour the SiC powder into ball mill and carry out wet ball mill, behind the thorough mixing, drying, half-dried molded, calcined 2-2.5 hour down at 980-1020 ℃, behind the stove naturally cooling, through the β phase silicon carbide aggregate of pulverizing, sieving and grading is prepared into the variable grain grade.
6, the method for preparation porous silicon carbide ceramic supporter as claimed in claim 1 is characterized in that add binding agent in ready-formed β phase silicon carbide aggregate powder, and add pore-forming material simultaneously, its concrete preparation method comprises following each step:
(1) raw material combination treatment: in ready-formed aggregate β phase silicon carbide powder, add binding agent and pore-forming material, be made into mixed powder, add deionized water and be made into slurry;
(2) with behind the slurry ball milling of step 1 at high temperature drying obtain powder, sieve dry-pressing or cold isostatic compaction;
(3) powder after the moulding is carried out pressureless sintering, sintering temperature is 1280-1360 ℃, and soaking time 2-6 hour, atmosphere was oxidizing atmosphere, gets the porous silicon carbide ceramic supporter with the stove naturally cooling.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009140791A1 (en) * | 2008-05-21 | 2009-11-26 | Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences | Process for producing silicon carbide |
| CN101913873A (en) * | 2010-08-03 | 2010-12-15 | 清华大学 | Method for making support body of porous ceramic filter pipe capable of improving strength and pore connectivity |
| CN101913874A (en) * | 2010-08-03 | 2010-12-15 | 清华大学 | Method for pretreating ceramic aggregates of porous ceramic filtering pipe support for high-temperature dust removal |
| CN101391181B (en) * | 2008-10-21 | 2011-04-06 | 南京工业大学 | Method for preparing porous ceramic film support |
| CN101318808B (en) * | 2007-08-07 | 2012-05-30 | 江苏省宜兴非金属化工机械厂 | Porous ceramic supporting body for high-strength inorganic separation film |
| CN102617179A (en) * | 2012-04-10 | 2012-08-01 | 清华大学 | Porous ceramic carrier for high-temperature and high-pressure inorganic filtering membrane and preparation method for porous ceramic carrier |
| CN102653474A (en) * | 2012-04-09 | 2012-09-05 | 南京工业大学 | Method for preparing high-porosity porous ceramic membrane support |
| CN109310953A (en) * | 2016-06-20 | 2019-02-05 | 欧洲技术研究圣戈班中心 | Filter comprising the separating layer based on β-SIC |
| CN113952918A (en) * | 2020-07-21 | 2022-01-21 | B·文 | Preparation method of adsorption material for evaporator |
-
2006
- 2006-01-13 CN CN 200610011191 patent/CN1793040A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101318808B (en) * | 2007-08-07 | 2012-05-30 | 江苏省宜兴非金属化工机械厂 | Porous ceramic supporting body for high-strength inorganic separation film |
| WO2009140791A1 (en) * | 2008-05-21 | 2009-11-26 | Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences | Process for producing silicon carbide |
| CN101391181B (en) * | 2008-10-21 | 2011-04-06 | 南京工业大学 | Method for preparing porous ceramic film support |
| CN101913873A (en) * | 2010-08-03 | 2010-12-15 | 清华大学 | Method for making support body of porous ceramic filter pipe capable of improving strength and pore connectivity |
| CN101913874A (en) * | 2010-08-03 | 2010-12-15 | 清华大学 | Method for pretreating ceramic aggregates of porous ceramic filtering pipe support for high-temperature dust removal |
| CN101913874B (en) * | 2010-08-03 | 2013-01-30 | 清华大学 | Method for pretreating ceramic aggregates of porous ceramic filtering pipe support for high-temperature dust removal |
| CN102653474A (en) * | 2012-04-09 | 2012-09-05 | 南京工业大学 | Method for preparing high-porosity porous ceramic membrane support |
| CN102617179A (en) * | 2012-04-10 | 2012-08-01 | 清华大学 | Porous ceramic carrier for high-temperature and high-pressure inorganic filtering membrane and preparation method for porous ceramic carrier |
| CN102617179B (en) * | 2012-04-10 | 2013-06-05 | 清华大学 | Preparation method of porous ceramic carrier for high-temperature and high-pressure inorganic filtering membrane |
| CN109310953A (en) * | 2016-06-20 | 2019-02-05 | 欧洲技术研究圣戈班中心 | Filter comprising the separating layer based on β-SIC |
| CN109310953B (en) * | 2016-06-20 | 2022-03-29 | 欧洲技术研究圣戈班中心 | Filter comprising a beta-SIC based separation layer |
| CN113952918A (en) * | 2020-07-21 | 2022-01-21 | B·文 | Preparation method of adsorption material for evaporator |
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