CN102617179B - Preparation method of porous ceramic carrier for high-temperature and high-pressure inorganic filtering membrane - Google Patents
Preparation method of porous ceramic carrier for high-temperature and high-pressure inorganic filtering membrane Download PDFInfo
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- CN102617179B CN102617179B CN 201210103839 CN201210103839A CN102617179B CN 102617179 B CN102617179 B CN 102617179B CN 201210103839 CN201210103839 CN 201210103839 CN 201210103839 A CN201210103839 A CN 201210103839A CN 102617179 B CN102617179 B CN 102617179B
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Abstract
The invention discloses a porous ceramic carrier for a high-temperature and high-pressure inorganic filtering membrane and a preparation method for the porous ceramic carrier. The porous silicon carbide ceramic carrier is prepared by silicon carbide, a binding agent and a pore-forming agent, wherein the mass ratio of the silicon carbide to the binding agent is 80-90:10-20, and the utilization quantity of the pore-forming agent is 35-45% of the sum of the volumes of the silicon carbide, the binding agent and the pore-forming agent. The preparation method includes adding the binding agent and the pore-forming agent in silicon carbide powder; performing ball milling, drying and vacuum heat casting forming; and performing pressureless sintering for a formed blank. Sintering temperature ranges from 1250 DEG C to 1350 DEG C, and heat insulation time ranges from 2 hours to 4 hours. As raw materials form main materials by means of fine size grading, the binding agent and the pore-forming agent are added by a special process, technologies such as unique vacuum heat casting forming and the like are adopted, and mechanical strength and porosity of the porous carrier can be improved effectively. The prepared silicon carbide porous ceramic carrier has excellent performances of fine thermal shock resistance, low coefficient of thermal expansion, fine mechanical and chemical stability at high temperature and under high pressure, and the like.
Description
Technical field
The present invention relates to a kind of High Temperature High Pressure inorganic filter film cellular ceramic substrate and preparation method thereof.
Background technology
Along with showing especially of energy problem, comprehensive effectively utilization of coal becomes more and more important.In the utilization of coal, a key issue that needs to solve is the high temperature filtration dedusting technology, and the pyroceramic filtering membrane is considered to address this problem the most effective approach.Cover one or more layers film on cellular ceramic substrate, just formed so-called ceramic filter membrane pipe.The outstanding advantages such as that ceramic membrane has is high temperature resistant, corrosion-resistant, resistance to erosion, physical strength is large, Stability Analysis of Structures is indeformable, the life-span is long, thereby be to be widely accepted, and sung the praises of the optimal selection into the hot particle filtering material.Mould material as a class novel green science and technology, the pyroceramic filtering membrane tube has a series of characteristics compared with high-polymer membrane: Heat stability is good, and chemical stability is good, and intensity is high, Mechanical Builds is stable, can carry out the regenerative operations such as the cleaning of soda acid or hot steam, high pressure recoil.
Yet due to inorganic ceramic filter membranous crisp, elasticity is little, frangible, they must be attached to therefore that the matrix (carrier) with certain physical strength is upper to be used.Thereby just must have good porosity, physical strength, unreactiveness, with teleblem, good associativity arranged, be difficult for taking off with teleblem under High Temperature High Pressure and strong corrosive environment and split as carrier.So to some degree, the selection of carrier and preparation are the bases of pyroceramic filtering membrane research.Because carborundum porous ceramics has that the coefficient of expansion is low, characteristics such as good machinery and chemical stability under good thermal shock, high temperature, its carrier as the inorganic filter film is widely used in the separating and filtering aspect of support of the catalyst and gas solid separation and molten metal.So carborundum porous ceramics just becomes the preferred material of pyroceramic filtering membrane tube carrier.
Preparation inorganic filter film porous silicon carbide ceramic carrier, the present means that usually adopt extrusion forming both at home and abroad.For the shorter carrier of size, such forming method a kind of ideal selection of can yet be regarded as; But for the length carrier that has certain requirements, limitation has just appearred in this method.At first, extrude goods in sintering process, due to length, the phenomenon of fracture often occurs, cause yield rate very low; Secondly, due to the consistence that can not guarantee the entire body raw material, thus even fracture do not occur in the situation that carrier burns till, also can't guarantee the consistence of overall mechanical strength, and can't satisfy the requirement of long period use.
Summary of the invention
The purpose of this invention is to provide a kind of under the High Temperature High Pressure environment for use, inorganic filter film with desirable chemical stability, intensity and suitable pore size distribution, porosity is with cellular ceramic substrate and preparation method thereof.
Porous silicon carbide ceramic carrier provided by the present invention is made by major ingredient silicon carbide, auxiliary material wedding agent and pore-forming material, wherein, the mass ratio of described silicon carbide and wedding agent is 80～90: 10～20, and the volume fraction of described pore-forming material is 35～45% of described silicon carbide, wedding agent and pore-forming material volume sum.
Wherein, described major ingredient silicon carbide is the silicon carbide of fine particle size classification, and its median size can be 250～300 μ m.
The silicon carbide major ingredient of this fine particle size classification specifically can prepare by following method: certain particle diameter (250～300 μ m) SiC powder is poured in Ceramic cylinder block, first passed through H
2SO
4Fully pickling, then pass through the abundant alkali cleaning of NaOH, at 100～200 ℃ of complete dryinies, be prepared into the silicon carbide major ingredient of required grain diameter grade through strict sieving and grading.
Described wedding agent specifically can be comprised of phases such as clay, kaolin and feldspars, and wherein, the mass ratio of clay, kaolin and feldspar is followed successively by 4～8: 4～8: 2～4.
It is 60～100 μ m, content higher than 90% following substances that described pore-forming material specifically can be median size: activated carbon, camwood knag or coke powder.
The preparation method of porous silicon carbide ceramic carrier of the present invention comprises the steps:
1) add wedding agent and pore-forming material in silicon carbide powder, be made into mixed powder; Add deionized water to be made into slurry in described mixed powder;
2) with step 1) the slurry ball milling mix after, cross 60 mesh sieves after spray-dried granulation or pressure-filteration drying and obtain powder; Powder is adopted the Vacuum Heat type casting moulding, make base substrate;
3) base substrate is carried out pressureless sintering, after cooling described porous silicon carbide ceramic carrier.
Wherein, step 3) described in, sintering carries out in air atmosphere, and the temperature of described sintering is 1250～1350 ℃, soaking time 2～4 hours.
The proportioning of mixed powder step 1) and deionized water is 1: 1.5～2.0.
The time of ball milling step 2) is 12～24 hours.
Due to the fine particle size classification formation major ingredient of the present invention through sic raw material, utilize special warfare to add wedding agent and pore-forming material, and adopt unique technology such as Vacuum Heat type casting moulding, can greatly improve intensity and the porosity of porous support.Prepared carborundum porous ceramics have good thermal shock, the coefficient of expansion low, have Good All-around Properties such as good machinery and chemical stability under High Temperature High Pressure.The inorganic filter film for preparing on this porous silicon carbide propping material has that porosity is high, hardness is high, the characteristics such as chemical transformation do not occur in wear-resisting and working process, thereby from material reduced that the inorganic filter film in use occurs because high temperature wear, hardness descend, fragility causes greatly the probability that lost efficacy, improved work-ing life and the result of use of inorganic filter film.Adopt in addition the pressureless sintering method to improve simultaneously the production efficiency of cellular ceramic substrate, reduced production cost.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described further, but the present invention is not limited thereto.
Experimental technique described in following embodiment if no special instructions, is ordinary method; Described reagent and material if no special instructions, all can obtain from commercial channels.
Fine particle size classification silicon carbide major ingredient used in following embodiment is prepared by the following method:
Certain particle diameter (250～300 μ m) SiC powder is poured in Ceramic cylinder block, first passed through H
2SO
4Fully pickling, then pass through the abundant alkali cleaning of NaOH, at 100～200 ℃ of complete dryinies, be prepared into through strict sieving and grading the silicon carbide major ingredient that median size is 250～300 μ m variable grain grades.
Embodiment one:
Be 280 μ m silicon carbide major ingredients with 88 gram median sizes, the activated carbon of 12 gram wedding agents (clay 5g, kaolin 4g, feldspar 3g) and volume fraction 40% (median size 90 μ m) mixes, pour into and carried out ball milling in the 200ml deionized water 24 hours, slurry is granulation in spray-drying tower.By the required powder that takes corresponding weight of reality, cast onto in steel die by Vacuum Heat, the round tube type base substrate is made in pressurization, cooling.Base substrate is put into stove with the corundum crucible of buried powder, under air atmosphere, burns till under the condition of 1300 ℃ of insulation 4h, with the stove naturally cooling, obtains the porous silicon carbide ceramic carrier.
Test result: the porosity of the SiC cellular ceramic substrate of preparation is 43%, and mean pore size is 55 μ m, and ultimate compression strength reaches 28MPa.Can guarantee under the High Temperature High Pressure working conditions requirement to carrier fully.
Wherein, porosity is with reference to the testing method in GB/T 1966-1996 standard; Ultimate compression strength is with reference to the testing method in the GB/T1964-1996 standard.
Embodiment two:
Be 250 μ m silicon carbide major ingredients with 80 gram median sizes, 20 gram wedding agents (clay 8g, kaolin 8g, feldspar 4g) and volume fraction 35% camwood knag (median size 100 μ m) mix, pour into and carried out ball milling in the 180ml deionized water 12 hours, slurry is granulation in spray-drying tower.By the required powder that takes corresponding weight of reality, cast onto in steel die by Vacuum Heat, the round tube type base substrate is made in pressurization, cooling.Base substrate is put into stove with the corundum crucible of buried powder, under air atmosphere, burns till under the condition of 1250 ℃ of insulation 3h, with the stove naturally cooling, obtains the porous silicon carbide ceramic carrier.
Test result: the porosity of the SiC cellular ceramic substrate of preparation is 45%, and mean pore size is 57 μ m, and ultimate compression strength reaches 23MPa.Can guarantee under the High Temperature High Pressure working conditions requirement to carrier fully.
Embodiment three:
Be 300 μ m silicon carbide major ingredients with 90 gram median sizes, 10 gram wedding agents (clay 4g, kaolin 3g, feldspar 3g) and volume fraction 42% coke powder (median size 60 μ m) mix, pour into and carried out ball milling in the 220ml deionized water 16 hours, slurry is by crossing 60 mesh sieves after pressure-filteration drying.By the required powder that takes corresponding weight of reality, cast onto in steel die by Vacuum Heat, the round tube type base substrate is made in pressurization, cooling.Base substrate is put into stove with the corundum crucible of buried powder, under air atmosphere, burns till under the condition of 1350 ℃ of insulation 2h, with the stove naturally cooling, obtains the porous silicon carbide ceramic carrier.
Test result: the porosity of the SiC cellular ceramic substrate of preparation is 38%, and mean pore size is 46 μ m, and ultimate compression strength reaches 35MPa.Can guarantee under the High Temperature High Pressure working conditions requirement to carrier fully.
Embodiment four:
Be 270 μ m silicon carbide major ingredients with 83 gram median sizes, 17 gram wedding agents (clay 8g, kaolin 5g, feldspar 4g) and volume fraction 43% activated carbon (median size 75 μ m) mix, pour into and carried out ball milling in the 235ml deionized water 20 hours, slurry is granulation in spray-drying tower.By the required powder that takes corresponding weight of reality, cast onto in steel die by Vacuum Heat, the round tube type base substrate is made in pressurization, cooling.Base substrate is put into stove with the corundum crucible of buried powder, under air atmosphere, burns till under the condition of 1320 ℃ of insulation 4h, with the stove naturally cooling, obtains the porous silicon carbide ceramic carrier.
Test result: the porosity of the SiC cellular ceramic substrate of preparation is 46%, and mean pore size is 53 μ m, and intensity reaches 26.6MPa.Can guarantee under the High Temperature High Pressure working conditions requirement to carrier fully.
Claims (4)
1. method for preparing the porous silicon carbide ceramic carrier, described porous silicon carbide ceramic carrier, made by silicon carbide, wedding agent and pore-forming material, wherein, the mass ratio of described silicon carbide and wedding agent is 80～90: 10～20, and the volume fraction of described pore-forming material is 35～45% of described silicon carbide, wedding agent and pore-forming material volume sum;
Comprise the steps:
1) add described wedding agent and pore-forming material in described silicon carbide, be made into mixed powder; Add deionized water to be made into slurry in described mixed powder;
2) with step 1) the slurry ball milling mix after, cross 60 mesh sieves after spray-dried granulation or pressure-filteration drying and obtain powder; Powder is adopted the Vacuum Heat type casting moulding, make base substrate;
3) described base substrate is carried out pressureless sintering, after cooling described porous silicon carbide ceramic carrier.
2. method according to claim 1, is characterized in that: step 3) described in sintering carry out in air atmosphere, the temperature of described sintering is 1250～1350 ℃, soaking time 2～4 hours.
3. method according to claim 1 and 2, it is characterized in that: described silicon carbide is the silicon carbide of fine particle size classification, its median size is 250～300 μ m.
4. method according to claim 1 and 2 is characterized in that: described pore-forming material is that median size is 60～100 μ m, active substance content higher than following any one material of 90%: activated carbon, camwood knag and coke powder.
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| CN102617179B true CN102617179B (en) | 2013-06-05 |
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| CN103011786B (en) * | 2012-12-03 | 2014-03-05 | 郑州振东科技有限公司 | Method for producing expanded ceramic heat-insulating plate by using shale and clinker |
| CN103539455B (en) * | 2013-10-09 | 2014-12-10 | 河南核净洁净技术有限公司 | High-temperature-resistant silicon carbide coated filter element for radioactive gas treatment and preparation method thereof |
| CN103819219B (en) * | 2014-01-22 | 2015-07-08 | 湖南大学 | Acid and alkali corrosion-resistant silicon carbide porous support |
| CN104261867B (en) * | 2014-09-23 | 2016-01-20 | 武汉工程大学 | A kind of preparation method of pure carborundum porous ceramics film |
| CN105254322A (en) * | 2015-11-04 | 2016-01-20 | 陕西科技大学 | Preparation method of oriented porous SiC ceramic with crystal boundary containing metal phases |
| CN106810290A (en) * | 2015-11-27 | 2017-06-09 | 衡阳凯新特种材料科技有限公司 | A kind of preparation method of carborundum porous ceramics |
| CN105330294B (en) * | 2015-12-01 | 2017-10-24 | 芜湖豫新世通汽车空调有限公司 | Filter membrane used for automobile air conditioning and preparation method thereof |
| CN105645986A (en) * | 2016-01-11 | 2016-06-08 | 梁小利 | High-bending-strength porous silicon carbide ceramic and preparation method thereof |
| CN108178655A (en) * | 2016-12-08 | 2018-06-19 | 辽宁法库陶瓷工程技术研究中心 | A kind of method added pore creating material technique and prepare silicon carbide ceramic filter |
| CN106631123B (en) * | 2017-01-10 | 2019-09-10 | 中国建筑材料科学研究总院 | A kind of honeycomb silicon carbide ceramics carrier and its preparation method and application |
| CN109534817B (en) * | 2017-09-21 | 2022-02-11 | 中南大学 | Preparation method of oriented porous structure of precursor conversion ceramic |
| CN108771912B (en) * | 2018-06-12 | 2020-11-24 | 山东华恩新材料科技有限公司 | Plate-type silicon carbide nano ceramic filter element and preparation method thereof |
| CN109650938A (en) * | 2019-01-16 | 2019-04-19 | 赵志刚 | Ceramic filter and its preparation method and application |
| CN110711494A (en) * | 2019-08-06 | 2020-01-21 | 北京中矿未来科技集团有限公司 | Tubular membrane assembly and system for purifying suspension liquid with high solid waste content |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1793040A (en) * | 2006-01-13 | 2006-06-28 | 清华大学 | Porous ceramic support for high strength inorganic separating film and preparation process thereof |
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| CN1793040A (en) * | 2006-01-13 | 2006-06-28 | 清华大学 | Porous ceramic support for high strength inorganic separating film and preparation process thereof |
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