CN101785944B - Preparation method of magnesium oxide ceramic foam filter for filtering magnesium and magnesium alloy melt - Google Patents
Preparation method of magnesium oxide ceramic foam filter for filtering magnesium and magnesium alloy melt Download PDFInfo
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- CN101785944B CN101785944B CN2010101218246A CN201010121824A CN101785944B CN 101785944 B CN101785944 B CN 101785944B CN 2010101218246 A CN2010101218246 A CN 2010101218246A CN 201010121824 A CN201010121824 A CN 201010121824A CN 101785944 B CN101785944 B CN 101785944B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention provides a magnesium oxide ceramic foam filter for filtering a magnesium and magnesium alloy melt and a preparation method thereof, relating to the field of metallurgy. The process is as follows: a polyurethane foam template is soaked in sodium hydroxide solution (10%) for 30 minutes under the temperature of 50 DEG C and is then washed by water and dried; electric-melting magnesium oxide, magnesium fluoride and water are mixed in a ball-milling manner according to the mass ratio so as to obtain water-based dispersion slurry; the polyurethane foam template is soaked in the slurry, and bisque is obtained through repeated slurry dipping and centrifugal slurry throwing; the bisque is put into an oven; finally, the dried bisque is put into a high-temperature furnace, is heated to1,200 to 1,300 DEG C at the speed of 1 to 3 DEG C/min, is heat-preserved for 2 hours, and is then naturally cooled in a furnace body. An obtained product of the invention has good chemical stability in the magnesium and the magnesium alloy melt, does not pollute the magnesium and the magnesium alloy melt, has good functions of absorbing and filtering nonmetallic inclusions in the magnesium and the magnesium alloy melt, and is suitable for filtering as well as purifying the magnesium and the magnesium alloy melt.
Description
Technical field
The present invention relates to field of metallurgy, particularly relate to a kind of method of production of ceramic foam filter, that is to say that related magnesia ceramic foam filter is applicable to the filtration, purification of magnesium and magnesium alloy fused mass.
Background technology
Magnesia ceramic foam filter has good 3 D stereo mesh skeleton structure, can filter various being mingled with and impurity in magnesium and the magnesium alloy liquation, improves the inherent quality of foundry goods and reduces defective.Magnesia ceramic foam filter has a extensive future in magnesium metal casting industry at present, but magnesia ceramic foam filter sintering temperature height, and power consumption is big, has limited its large-scale promotion and use.
Various inclusion defects in magnesium and the Mg alloy castings tend to cause cast properties to reduce even scrap, and become one of major obstacle of magnesium alloy extensive use, and this is because the chemical property of magnesium is very active, numerous materials such as O under the high temperature in meeting and the environment
2, H
2O, N
2Deng reacting, thereby cause in former magnesium production, magnesium alloy smelting and the process, unavoidably introduce many field trashes, thereby reduce the quality and the serviceability of magnesium alloy member, and the field trash in the magnesium alloy is mainly with magnesia, Mg
3N
2Deng nonmetallic substance is main, and wherein magnesia accounts for about 80% of nonmetallic inclusion, and it is very important for improving the quality of products therefore to remove magnesia impurity.
Using foamed ceramics that metal bath is filtered has had the history of decades, has invented ceramic slurries such as utilizing aluminium oxide, kaolin from the U.S. in 1978 and has successfully developed foamed ceramics, is used for after the aluminium alloy casting filtration, countries such as English, day, moral, Switzerland have competitively carried out research, have developed various material, are suitable for the ceramic foam filter of different purposes, as Al3O2, ZrO2, SiO2, Si3N4, high temperature foamed ceramicses such as boride, and for example United States Patent (USP) 3,990, and 901; 6,887,809, Chinese patent 97195118.7; 200510035623.3; Prepare the method for various foamed ceramicses 200710139287.6 disclose some Deng all, and the foam filter of these materials and be not suitable for magnesium and the filtration of magnesium alloy fused mass.This is because the activity of magnesium metal is very high, be very easy to as Al3O2, ZrO2, foamed ceramics matrix materials such as SiO2 react, and make the foamed ceramics corrode of above-mentioned material become harmful components among entering magnesium and magnesium alloy fused mass.Consider that from the angle of foamed ceramics chemical stability the foamed ceramics of materials such as magnesia and CaO is the filtration that is suitable as very much magnesium and magnesium alloy fused mass.Compare with magnesia, CaO moisture absorption tendency is bigger, the foamed ceramics that obtains needs the erosion of strict restriction water in depositing process, otherwise can cause product strength to descend even be difficult to using, unless adopt special means of defence, and such foamed ceramics needs strict high temperature drying to dewater just can to use before use, and is very inconvenient.Use magnesia ceramic foam then can avoid above-mentioned situation, and the magnesia impurity in magnesium and the magnesium alloy is had good adsorption and filtration, thermal capacitance is little, and resistance is little and filtration yield is big, and particularly need not preheating can directly use.
So far, the preparation process of all kinds of ceramic foam filters is roughly as follows:
Prepare foamed material template-preparation ceramic size-on template, apply slurry-drying-sintering of sizing mixing-obtain goods.Committed step in the preparation process is to select for use a kind of suitable decentralized medium that ceramic powder is disperseed, and makes slurry and just can be coated on the template.Yet water can be used for modulating Al
3O
2In the slurry of foamed ceramics, but can not be used for modulating the magnesia ceramics slurry, can there be following hydration reaction as making water modulate the magnesia slurry in the notification number CN1473947A Chinese patent:
Magnesia+H
2O=Mg (OH)
2
This will cause the magnesia slurry viscosity to increase and the solid content reduction, cause the magnesia amount of polyurethane foamed material surface absorption few.In addition, this slurry can lose the physical bond water of slurry about 110～130 ℃ in the heat drying process, at 340 ℃ of left and right sides Mg (OH)
2Dehydration can take place produce magnesia, continue heat-agglomerating and can obtain magnesia ceramic foam.Owing to be adsorbed on the continuous dehydration of slurry on the foamed material, can form a large amount of spaces, cause the final products porosity big, intensity is lower.
Notification number CN87102516A then replaces water to prepare the magnesia slurry with the ethanol solution of pure Novolac, thereby can avoid the magnesia hydration reaction, but absolute ethanol volatilizes speed is very fast, in the mechanical milling process, the high viscosity of alcohol Novolac will soon display, be difficult to obtain the magnesia slurry of high solids content under the described condition of patent, the distribution of magnesia slurry on the foam network also is difficult to evenly.
In addition, the sintering temperature of general pottery is about 0.6 of its raw material fusing point, and magnesian fusing point is 2852 ℃, and this makes that the sintering temperature of magnesia ceramic foam is very high.Chinese patent CN101138691 CN87102516 CN101164656 etc. based on the foamed ceramics sintering temperature of magnesia generally between 1450 ℃-1800 ℃, 1650 ℃ of temperature commonly used, sintering temperature is higher, it is huge to consume energy.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who is used for magnesium and magnesium alloy fused mass filtration usefulness magnesia ceramic foam filter, make the electrically molten magnesia slurry change the plasticity material into, can be good at adhering on the polyurethane foam template network, improve its adhesive capacity, thereby increase end article intensity.In raw material, add a spot of magnesium fluoride simultaneously as binding agent, make magnesia under lower sintering temperature, just can obtain desirable strength.
The objective of the invention is to be achieved through the following technical solutions:
Be used for magnesium and magnesium alloy fused mass and filter the preparation method who uses magnesia ceramic foam filter, this method realizes by following process:
(1) select the polyurethane foam template,,, take out it is soaked 30min in 50 ℃ the 10%NaOH aqueous solution after, wash nature with clear water and dry according to technological requirement cutting size such as 20PPI, standby;
(2) raw material of following mass percent: electrically molten magnesia 50～60, magnesium fluoride 10～20, the mixing of water 30～40 ball millings obtain even water base dispersion slurry;
(3) the polyurethane foam template of handling well is immersed among the slurry, by dipping in slurry repeatedly and centrifugal process of getting rid of slurry makes the electrically molten magnesia powder amount of adhesion reach technological requirement, obtain plain embryo, then place 80 ℃ baking oven to place 2h plain embryo, then be placed on again and place 2h in 120 ℃ the baking oven and carry out the moulding dehydration;
(4) will place high temperature furnace through the plain embryo that step (3) is handled, speed with 1～3 ℃/min is warming up between 1150-1250 ℃, and insulation 2h, in body of heater, cool off the magnesia ceramic foam filter that promptly obtains can be used for magnesium and magnesium alloy fused mass filtration, purification naturally.
The specific embodiment
Below the present invention is described in detail:
Light calcined magnesia (Magnesium oxide) is a kind of odorless, tasteless, nontoxic white unformed powder, fusing point is 2852 ℃, boiling point is 3600 ℃, this powder is through high temperature sintering more than 1000 ℃, begin to be converted into crystal, when temperature rises to more than 1500 ℃, just begin to be transformed into dead roasting magnesia or sintered magnesia, that is to say that being higher than this temperature can produce the magnesia ceramic foam that performance meets the demands.Sintering temperature is too high, and it is very big to consume energy, and in order to reduce energy resource consumption, reduces the discharge capacity of greenhouse gases, just needs to reduce the sintering temperature of magnesia ceramic foam, and we have added magnesium fluoride as the magnesia sintering binder for this reason.On the one hand, because the fusing point of magnesium fluoride is 1266 ℃, in the time of near being heated to fusing point, fusion can take place and the magnesium oxide particle on every side that bonds in it, after cooling can make magnesia be connected one with magnesium fluoride, becomes the very high sintered body of intensity; On the other hand, when sintering temperature reached near the magnesium fluoride fusing point, crystallization had taken place in magnesium oxide powder, forms bigger crystal grain, and this also will further improve the intensity of final products.
Secondly, prepare the used magnesia of magnesia ceramic foam at present based on light calcined magnesia, this magnesia activity is very high, is easy to and water generation hydration reaction.Under the normal temperature, the magnesia slip just begins to take place hydration reaction place about 2-3h in water after, and hydration reaction is exothermic reaction, and slurry temperature raises naturally, and vigorous reaction takes place when reaching 100 ℃, and this moment, reaction was very fast, and about 0.5-1h reacts completely.Particularly when summer temp was higher, hydration reaction was very fast, was reflected in the 0.5h to finish.And for magnesia and water are mixed, often need to use ball mill, frictional heat can further be accelerated hydration reaction speed during ball milling, and when replacing water as decentralized medium with lower boiling absolute ethyl alcohol, absolute ethyl alcohol is highly volatile in mechanical milling process, and adopt electrically molten magnesia under process conditions, then can avoid the generation of hydration reaction substantially.This be since light calcined magnesia in the high-temperature calcination process, along with temperature raises, the magnesia volume shrinks gradually, density increases, magnesia crystal is grown and is grown up, its institutional framework is more and more finer and close, forms the electrically molten magnesia that is difficult to water generation hydration reaction.In addition, electrically molten magnesia density is bigger, can reach 3.4, can effectively improve solid content of slurry, thereby reduces the space between the magnesium oxide particle, improves the compaction rate and the intensity of final products.
Embodiment 1
With aperture 10PPI, the polyurethane foam template of size 100 * 100 * 25mm immerses in 50 ℃ the 10%NaOH aqueous solution, takes out behind the 30min, and is removing the residual alkali lye of template surface, after dry naturally, standby with the clear water washing.Than the molten magnesia of power taking, magnesium fluoride and water also placed ball mill mixing 1h to obtain even water base dispersion slurry by 50: 10: 40 quality.Standby polyurethane template is made on the foam network and is stained with slurry, the plain embryo that makes by dipping in slurry-centrifugal process repeatedly in slurry.The plain embryo that then will make places 50 ℃ baking oven to dry 2h, continue dry 2h in 120 ℃ the baking oven and be placed on, at last plain embryo is placed high temperature furnace, be warming up to 1250 ℃ with the speed of 1 ℃/min and carry out sintering, and insulation 2h, natural cooling can obtain magnesia ceramic foam filter.
Embodiment 2
With aperture 20PPI, the polyurethane foam template of size Φ 200 * 25mm immerses in 50 ℃ the 10%NaOH aqueous solution, takes out behind the 30min, and is removing the residual alkali lye of template surface, after dry naturally, standby with the clear water washing.Than the molten magnesia of power taking, magnesium fluoride and water also placed ball mill mixing 1h to obtain even water base dispersion slurry by 50: 15: 35 quality.Standby polyurethane template is made on the foam network and is stained with slurry, the plain embryo that makes by dipping in slurry-centrifugal process repeatedly in slurry.The plain embryo that then will make places 50 ℃ baking oven to dry 2h, continue dry 2h in 120 ℃ the baking oven and be placed on, at last plain embryo is placed high temperature furnace, be warming up to 1300 ℃ with the speed of 3 ℃/min and carry out sintering, and insulation 2h, natural cooling can obtain magnesia ceramic foam filter.
The introduction that above-mentioned implementation example is detailed the magnesium metal filtration with the preparation method of magnesia ceramic foam filter, though only be to use an example, help understanding to principle of the present invention and implementation method.For being engaged in those skilled in the art, can on specific embodiment, change according to core concept of the present invention, so the content of this specification is not appreciated that limitation of the present invention.
Claims (1)
1. be used for magnesium and magnesium alloy fused mass and filter the preparation method who uses magnesia ceramic foam filter, it is characterized in that this method realizes by following process:
(1) select the polyurethane foam template, 20PPI according to technological requirement cutting size, takes out it is soaked 30min in 50 ℃ the 10%NaOH aqueous solution after, washs nature with clear water and dries, and is standby;
(2) raw material of following mass percent: electrically molten magnesia 50～60, magnesium fluoride 10～20, the mixing of water 30～40 ball millings obtain even water base dispersion slurry;
(3) the polyurethane foam template of handling well is immersed among the slurry, by dipping in slurry repeatedly and centrifugal process of getting rid of slurry makes the electrically molten magnesia powder amount of adhesion reach technological requirement, obtain plain embryo, then place 80 ℃ baking oven to place 2h plain embryo, then be placed on again and place 2h in 120 ℃ the baking oven and carry out the moulding dehydration;
(4) will place high temperature furnace through the plain embryo that step (3) is handled, speed with 1～3 ℃/min is warming up between 1150-1250 ℃, and insulation 2h, in body of heater, cool off the magnesia ceramic foam filter that promptly obtains can be used for magnesium and magnesium alloy fused mass filtration, purification naturally.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101218246A CN101785944B (en) | 2010-03-11 | 2010-03-11 | Preparation method of magnesium oxide ceramic foam filter for filtering magnesium and magnesium alloy melt |
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|---|---|---|---|
| CN2010101218246A CN101785944B (en) | 2010-03-11 | 2010-03-11 | Preparation method of magnesium oxide ceramic foam filter for filtering magnesium and magnesium alloy melt |
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| Publication Number | Publication Date |
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| CN101785944A CN101785944A (en) | 2010-07-28 |
| CN101785944B true CN101785944B (en) | 2011-12-21 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102121071A (en) * | 2011-01-10 | 2011-07-13 | 沈阳工业大学 | Magnesium oxide ceramic filter for purification of magnesium alloy melt |
| CN102898175A (en) * | 2012-10-17 | 2013-01-30 | 沈阳化工大学 | Technique for producing alumina foamed ceramic by gelcasting |
| CN103553686B (en) * | 2013-11-05 | 2015-04-29 | 中钢集团洛阳耐火材料研究院有限公司 | Magnesium aluminate spinel foamed ceramic filter as well as preparation method thereof |
| CN107285743B (en) * | 2016-03-30 | 2021-02-19 | 宝山钢铁股份有限公司 | Method for preparing porous ceramic from waste magnesium oxide |
| CN108439957B (en) | 2018-04-08 | 2020-04-21 | 凤阳爱尔思轻合金精密成型有限公司 | MA-M2T-spinel solid solution reinforced magnesium oxide base foamed ceramic filter and preparation method thereof |
| CN108484182B (en) | 2018-04-08 | 2020-05-01 | 江苏中翼汽车新材料科技有限公司 | Magnesium aluminate spinel reinforced magnesium oxide based foamed ceramic filter synthesized in situ by magnesium oxide whiskers and preparation method thereof |
| CN108503378B (en) | 2018-04-08 | 2020-06-05 | 江苏中翼汽车新材料科技有限公司 | Spinel reinforced magnesium oxide base foamed ceramic filter and preparation method thereof |
| CN116161981B (en) * | 2023-04-26 | 2023-08-22 | 山东硅元新型材料股份有限公司 | Preparation method of anhydrous magnesium oxide foam ceramic |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4257810A (en) * | 1978-08-12 | 1981-03-24 | Bridgestone Tire Company Limited | Cordierite, silica, alumina porous ceramic body |
| CN1410393A (en) * | 2002-11-21 | 2003-04-16 | 上海交通大学 | Preparation method of special foamed ceramic filter for magnesium alloy |
| CN1281771C (en) * | 2003-06-09 | 2006-10-25 | 李华伦 | Foamed ceramic for magnesium and magnesium alloy melt purification |
| CN101138691A (en) * | 2007-07-10 | 2008-03-12 | 济南圣泉倍进陶瓷过滤器有限公司 | Preparation method of magnesian foamed ceramic filter for casting |
-
2010
- 2010-03-11 CN CN2010101218246A patent/CN101785944B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4257810A (en) * | 1978-08-12 | 1981-03-24 | Bridgestone Tire Company Limited | Cordierite, silica, alumina porous ceramic body |
| CN1410393A (en) * | 2002-11-21 | 2003-04-16 | 上海交通大学 | Preparation method of special foamed ceramic filter for magnesium alloy |
| CN1281771C (en) * | 2003-06-09 | 2006-10-25 | 李华伦 | Foamed ceramic for magnesium and magnesium alloy melt purification |
| CN101138691A (en) * | 2007-07-10 | 2008-03-12 | 济南圣泉倍进陶瓷过滤器有限公司 | Preparation method of magnesian foamed ceramic filter for casting |
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