CN107628819A - A kind of method for the porous material that the phase containing melilite is prepared using magnesium slag, flyash, carbide slag - Google Patents
A kind of method for the porous material that the phase containing melilite is prepared using magnesium slag, flyash, carbide slag Download PDFInfo
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- CN107628819A CN107628819A CN201610564963.3A CN201610564963A CN107628819A CN 107628819 A CN107628819 A CN 107628819A CN 201610564963 A CN201610564963 A CN 201610564963A CN 107628819 A CN107628819 A CN 107628819A
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
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Abstract
The industrial solid castoff discharge capacity such as magnesium slag, flyash, carbide slag is big, takes large amount of land resources, and easily forms dust, causes air and water pollution.The method of the present invention prepares the porous material of the phase containing melilite using magnesium slag, flyash, carbide slag doping by high temperature sintering, the purpose of the treatment of wastes with processes of wastes against one another is not only reached, and obtained porous material, available for sound insulation, insulation, the fields such as filtering, the application field of industrial solid castoff recycling is expanded.
Description
Technical field
The present invention relates to a kind of method for the porous material that the phase containing melilite is prepared using industrial solid castoff, belong to pottery
Ceramic material field.
Background technology
A kind of mineral in the silicates mineral that melilite is made up of calcium silicates/sodium metasilicate containing aluminium, magnesium, iron, change
Study a point formula (Ca, Na)2(Al,Mg,Fe2+)[(Al,Si)SiO7].Cacoclasite Ca2Al(AlSi)O7And akermanite
(Ca2Mg(Si2O7) it is two kinds of most important mineral in melilite race, in composition, replaced between Mg-Al for perfect isomorphism, together
When with the replacement between Si-Al, therefore formed with cacoclasite and the isomorphic replacement of akermanite.These mineral be from
Crystallized in alkaline magma rich in calcium.
Melilite is mainly used in the manufacturing fields such as ceramic glaze, ceramics, refractory material, insulation material and cement.In addition
Akermanite Ca2Mg(Si2O7) be that one kind contains Si, Ca, Mg ceramics, there is bioactivity, have in bioengineered tissue compared with
Good application prospect.
At present, large-scale industry is mainly derived from ore extraction with melilite, there is larger ecology and environmental disruption hidden danger.
Fine chemistry industry is mainly prepared with melilite using sol-gal process and the precipitation method, and raw materials used is chemically pure reagent, Wu Faman
Foot large-scale production and application.
And on the other hand, China discharges substantial amounts of flyash and various industrial slags every year, covers soil, pollution environment and
Increase investment, these discarded objects are made full use of to be developed a circular economy, building a conservation-minded society has to improving the level of resources utilization
Highly important meaning.But current China industrial solid castoff recycles mainly to be filled with temporary road and terrace, sintering system
The mode of the simple reprocessing processing such as standby clinker, sintering brickmaking utilizes, the species for the industrial solid castoff being utilized
It is all very limited with the scope of application of generation product.
The main chemical of flyash is SiO2、Al2O3、CaO、MgO、TiO2, sulfide etc..Magnesium slag is refining magnesium discharge
A kind of industrial residue, main chemical compositions CaO, SiO2、Al2O3Deng.Carbide slag be calcium carbide prepare obtain after acetylene with hydrogen
Calcium oxide is the solid slag of main component, while also contains SiO2、Al2O3And a small amount of CaCO3、Fe2O3, MgO, carbon slag etc. it is miscellaneous
Matter.
Understanding according to inventor, the relevant report using industrial solid castoff manufacture ceramics or refractory material is fewer,
The research that magnesium slag, carbide slag the like waste recycle in Industrial Solid Waste is nor a lot.
Chinese patent application CN201210258832.4 disclose using industrial residue magnesium slag, kaolin and commercial alumina as
Raw material, the method that calcium hexaluminate/anorthite complex phase light heat insulating refractory materials are prepared by pyroreaction sintering process should
Preparation method realizes the comprehensive utilization of magnesium slag to a certain extent, and its material has high temperature resistant, lightweight, the spy of heat-insulation and heat-preservation
Point, it is applicable to the liner high-temperature material of elevated temperature vessel and kiln.But this method has only digested a kind of industrial residue, kaolinite used
Soil and commercial alumina still come from ore and industrial production.
Chinese patent application CN201410581205.3 discloses a kind of magnesium slag and manganese slag castable refractory raw material, is a kind of
Unshape refractory, including 20~30 parts of aggregates, 70~80 parts of powders, 10~15 parts of additives, the aggregate is by corundum, magnesium
Aluminate forms；The powder is by α-Al2O3Powder, magnesium ground-slag, flyash, manganese ground-slag composition；The additive is water-soluble phenolic
Urea formaldehyde.Generation hydrated calcium silicate gel is formed after magnesium ground-slag mixes with water soluble phenol resin in the invention, can be improved
The curing rate of magnesium slag and manganese slag castable refractory.Although the preparation method has digested three kinds of Industrial Solid Wastes, but Industrial Solid used
Useless ratio is still less high.
The content of the invention
In view of the research that ceramic material is manufactured during industrial solid castoff recycles at present is few, to magnesium slag, flyash, electricity
The comprehensive utilization of three kinds of solid waste of rock ballast is insufficient, and the present invention is in further investigation magnesium slag, flyash, carbide slag ingredient properties
On the basis of, it is proposed that the method that the porous material for preparing the phase containing melilite is adulterated by these three solid waste, on the one hand solve
Certainly the problem of the treatment of wastes with processes of wastes against one another, on the one hand provide available for be incubated, the porous material of the phase containing melilite of sound insulation or filtering etc.
Material.
Technical scheme is as follows：
A kind of preparation method of the porous material of the phase containing melilite：Magnesium slag, flyash, carbide slag are mixed, the mixing
Thing is compressing, sinters afterwards.
Preferably magnesium slag:Flyash:The mass ratio of carbide slag is 1:0.0625~0.8:0.0625~0.7, further preferably
For 1:0.25~0.8:0.07~0.5, more preferably 1:0.35~0.8:0.07~0.35, most preferably 1:0.4~0.6:
0.15~0.3.
The condition for being preferably laminated to type is：Briquetting pressure is 60MPa~110MPa, more preferably 78MPa~
98MPa.Dwell time is 50~80s.
As well known to those skilled in the art, conventional various pressure forming methods are used equally for the present invention, include but is not limited to,
Cold isostatic compaction, compression molding etc..It is preferred that use compression molding.
It is preferred that sintering condition is：Heating rate is 5-15 DEG C/min, and sintering temperature is 1100~1200 DEG C, and soaking time is
3-5 hours.More preferably heating rate is 9-11 DEG C/min, soaking time 210-270min.
It is preferred that sintering processing sinters for high temperature pressure-free.
It is preferred that magnesium slag, flyash and carbide slag can be crushed before combination, or crushed in mixing.It is preferred that make
The particle diameter of magnesium slag, flyash and carbide slag is at 1~100 μm in mixture, more preferably 5~50 μm.
As well known to those skilled in the art, conventional breaking method can be used in the present invention, include but is not limited to：Extrude powder
Broken, extruding-shearing crushes, cleaves crushing, impact comminution etc., and the reducing mechanism that can be used includes but is not limited to：Jaw crushing
Machine, post mill, Raymond mill, Ball Mill, Vertical Mill, rod milling, punching rotation disintegrating machine, hammer mill etc..
The present invention also provides the porous material of the phase containing melilite prepared by above-mentioned preparation method.
It is preferred that the porous material of the phase containing melilite, its total porosity is 19%~57%, bulk density is 1.38~
2.15g/cm3, water absorption rate is 8.9%~34.5%, and compression strength is 0.8MPa~98.4MPa.
The total porosity of the porous material of the further preferably described phase containing melilite is 25%~42%；It is preferred that its volume is close
Spend for 1.63~1.90g/cm3；It is preferred that its water absorption rate is 15.0%~25.5%；It is preferred that its compression strength be 10.0MPa~
63.0MPa。
Term " total porosity " used refers to closed porosity and apparent porosity sum in the present invention.
The quality that term " bulk density " used is porous materialses without free water in the present invention and its cumulative volume (including
The reality of material accounts for volume shared by volume and whole holes) ratio.
In the present invention term " water absorption rate " used be in porous materialses the quality for the water that all open pores are absorbed with
The mass ratio value of its drying material.
Wherein the assay method of total porosity, bulk density and water absorption rate uses Archimedes method.
Advantages of the present invention：
Three kinds of magnesium slag, flyash, carbide slag repressed sintering of solid waste, SiO therein2、Al2O3, CaO, MgO etc.
Constitutional changes form melilite phase, such as akermanite (Ca2Mg(Si2O7)) and/or cacoclasite (Ca2MgxAlx(SixAlx)
O7) phase, form the material containing melilite phase, there is provided a kind of melilite phase material for substituting ore source.
In addition, carbonaceous remaining in flyash and carbide slag, calcium carbonate, calcium hydroxide, generates CO in sintering process2,
The stomata burnt till in material is formed, is not required to additionally add pore creating material, makes full use of the compositing characteristic of each Industrial Solid Waste, reduce and match somebody with somebody
The complexity of material, and substantially increase ratio of the Industrial Solid Waste in dispensing.
The porous material of the obtained phase containing melilite, according to its total porosity, bulk density and compression strength, depending on use
Condition requirement, available for sound insulation, insulation, filtering etc., the application field that Industrial Solid Waste recycles product is widened.For example,
Filter it is less demanding to the compression strength of material therefor, when the porous material of the phase prepared according to the methods of the invention containing melilite,
When total porosity and higher water absorption rate, filtering material can be used as；Sound insulation or insulation require higher to the compression strength of material therefor,
When the porous material of the phase prepared according to the methods of the invention containing melilite, compression strength in more than 10MPa, can be used as sound insulation or
Insulation material.
Brief description of the drawings
XRD comparison diagrams before and after the magnesium slags of Fig. 1 embodiments 1, flyash, carbide slag mixture sintering
Microcosmic porous shape appearance figure after the magnesium slags of Fig. 2 embodiments 1, flyash, carbide slag mixture sintering
Microcosmic porous shape appearance figure after the magnesium slags of Fig. 3 embodiments 2, flyash, carbide slag mixture sintering
XRD after the magnesium slags of Fig. 4 embodiments 3, flyash, carbide slag mixture sintering
XRD after the magnesium slags of Fig. 5 embodiments 5, flyash, carbide slag mixture sintering
Embodiment
The porous material compressive property of the phase containing melilite is measured using SANS-CMT5350 section bar material universal testing machine；Material
Total porosity, bulk density, water absorption rate using Archimedes method measure；The thing of material mutually uses Japanese Shimadzu XRD-6000 types
X-ray diffractometer is analyzed；The loose structure of material uses electron microscope observation.
The mixing of magnesium slag, flyash, carbide slag shakes magnesium after ball milling using Rigaku-9306D models concussion ball mill
Slag, flyash, the particle diameter of carbide slag are 4-50 μm.
The a diameter of 20mm of compression molding mould therefor.Briquetting pressure is 64MPa~100MPa；Dwell time is 50~60s
Left and right.For ease of carrying out Mechanics Performance Testing, control sample size height is in 20 ± 1mm.
Embodiment 1
Specific steps：
(1) three kinds of magnesium slag, flyash, carbide slag solid waste are according to mass ratio 1：0.5：0.17 takes 200g；
(2) three kinds of slag charges are mixed with concussion ball mill, incorporation time 60s；
(3) well mixed powder is positioned over compression molding among mould, briquetting pressure 95.9MPa, dwell time
For 60s；
(4) sample after shaping is positioned over progress high temperature pressure-free sintering in Muffle furnace, heating rate is 10 DEG C/min, sintering
Temperature is 1150 DEG C, soaking time 240min, and sintering is completed, and is statically placed in natural cooling in Muffle furnace；
(5) sample carries out subsequent analysis test.
Surveyed compression strength is 29.97MPa, total porosity 33.72%, water absorption rate 20.10%, and bulk density is
1.68g/cm3.XRD material phase analysis, and its porous microscopic appearance are shown in attached Fig. 1 and 2.
Embodiment 2
Specific steps：
(1) three kinds of magnesium slag, flyash, carbide slag solid waste are according to mass ratio 1：0.36：0.07 takes 200g；
(2) three kinds of slag charges are mixed with concussion ball mill, incorporation time 60s；
(3) well mixed powder is positioned over compression molding among mould, briquetting pressure 95.9MPa, dwell time
For 60s；
(4) sample after shaping is positioned over progress high temperature pressure-free sintering in Muffle furnace, heating rate is 10 DEG C/min, sintering
Temperature is 1150 DEG C, soaking time 240min, and sintering is completed, and is statically placed in natural cooling in Muffle furnace；
(5) sample carries out subsequent analysis test.
Surveyed compression strength is 98.36MPa, total porosity 19.6%, water absorption rate 8.92%, and bulk density is
2.09g/cm3.Its microstructure is as shown in Figure 3.
Embodiment 3
Specific steps：
(1) three kinds of magnesium slag, flyash, carbide slag solid waste are according to mass ratio 1：0.42：0.25 takes 200g；
(2) three kinds of slag charges are mixed with concussion ball mill, incorporation time 60s；
(3) well mixed powder is positioned over compression molding among mould, briquetting pressure 95.5MPa, dwell time
For 60s；
(4) sample after shaping is positioned over progress high temperature pressure-free sintering in Muffle furnace, heating rate is 10 DEG C/min, sintering
Temperature is 1150 DEG C, soaking time 240min, and sintering is completed, and is statically placed in natural cooling in Muffle furnace；
(5) sample carries out subsequent analysis test.
Surveyed compression strength is 20.70MPa, total porosity 33.74%, water absorption rate 18.97%, and bulk density is
1.79g/cm3.Its XRD material phase analysis is as shown in Figure 4.
Embodiment 4
Specific steps：
(1) three kinds of magnesium slag, flyash, carbide slag solid waste are according to mass ratio 1：0.25：0.42 takes 200g；
(2) three kinds of slag charges are mixed with concussion ball mill, incorporation time 60s；
(3) well mixed powder is positioned over compression molding among mould, briquetting pressure 95.5MPa, dwell time
For 60s；
(4) sample after shaping is positioned over progress high temperature pressure-free sintering in Muffle furnace, heating rate is 10 DEG C/min, sintering
Temperature is 1150 DEG C, soaking time 240min, and sintering is completed, and is statically placed in natural cooling in Muffle furnace；
(5) sample carries out subsequent analysis test.
Surveyed compression strength is 0.87MPa, total porosity 56.96%, water absorption rate 34.32%, and bulk density is
1.66g/cm3。
Embodiment 5
Specific steps：
(1) three kinds of magnesium slag, flyash, carbide slag solid waste are according to mass ratio 1：0.8：0.2 takes 200g；
(2) three kinds of slag charges are mixed with concussion ball mill, incorporation time 60s；
(3) well mixed powder is positioned over compression molding among mould, briquetting pressure 95.5MPa, dwell time
For 60s；
(4) sample after shaping is positioned over progress high temperature pressure-free sintering in Muffle furnace, heating rate is 10 DEG C/min, sintering
Temperature is 1150 DEG C, soaking time 240min, and sintering is completed, and is statically placed in natural cooling in Muffle furnace；
(5) sample carries out subsequent analysis test.
Surveyed compression strength is 32.47MPa, total porosity 28.98%, water absorption rate 16.10%, and bulk density is
1.80g/cm3.Its XRD material phase analysis is as shown in Figure 5.
Claims (8)
- A kind of 1. preparation method of the porous material of phase containing melilite, it is characterised in that：Magnesium slag, flyash, carbide slag are mixed, The mixture is compressing, sinters afterwards.
- 2. preparation method as claimed in claim 1, it is characterised in that：Magnesium slag:Flyash:The mass ratio of carbide slag is 1: 0.0625~0.8:0.0625~0.7, more preferably 1:0.25~0.8:0.07~0.5, more preferably 1:0.35~ 0.8:0.07~0.35, most preferably 1:0.4~0.6:0.15~0.3.
- 3. preparation method as claimed in claim 1 or 2, it is characterised in that：Briquetting pressure is 60MPa~110MPa, further Preferably 78MPa~98MPa.Dwell time is 50~80s.
- 4. the preparation method as described in claim any one of 1-3, it is characterised in that：Sintering heating rate is 5-15 DEG C/min, Sintering temperature is 1100~1200 DEG C, and soaking time is 3-5 hours.It is preferred that heating rate is 9-11 DEG C/min, soaking time is 210-270min。
- 5. the preparation method as described in claim any one of 1-4, it is characterised in that：Magnesium slag, flyash, carbide slag in mixture Particle diameter be 1-100 μm, preferably 5-50 μm.
- A kind of 6. porous material of phase containing melilite, it is characterised in that：Using the preparation method described in claim any one of 1-5 Prepare.
- 7. the porous material of the phase containing melilite as claimed in claim 6, it is characterised in that Archimedes method determines, total stomata Rate is 19%~57%, and bulk density is 1.38~2.15g/cm3, water absorption rate is 8.9%~34.5%, and compression strength is 0.8MPa~98.4MPa.
- 8. the porous material of the phase containing melilite as claimed in claim 7, it is characterised in that the porous material of the phase containing melilite The total porosity of material is 25%~42%, and bulk density is 1.63~1.90g/cm3, water absorption rate is 15.0%~25.5%, is resisted Compressive Strength is 10.0MPa~63.0MPa.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558361A (en) * | 2018-05-25 | 2018-09-21 | 北方民族大学 | The porosity adjustable porous ceramics and preparation method prepared with flyash, carbide slag |
| CN108756107A (en) * | 2018-06-27 | 2018-11-06 | 燕翔 | It is a kind of that sand abatvoix is covered based on mineral wool |
| CN113636835A (en) * | 2021-08-30 | 2021-11-12 | 武汉理工大学 | Anorthite heat storage ceramic prepared from magnesium slag and preparation method thereof |
| CN114920578A (en) * | 2022-07-20 | 2022-08-19 | 淄博金狮王科技陶瓷集团有限公司 | Preparation method of porous anorthite/gehlenite complex-phase ceramic with low sintering shrinkage |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558361A (en) * | 2018-05-25 | 2018-09-21 | 北方民族大学 | The porosity adjustable porous ceramics and preparation method prepared with flyash, carbide slag |
| CN108756107A (en) * | 2018-06-27 | 2018-11-06 | 燕翔 | It is a kind of that sand abatvoix is covered based on mineral wool |
| CN113636835A (en) * | 2021-08-30 | 2021-11-12 | 武汉理工大学 | Anorthite heat storage ceramic prepared from magnesium slag and preparation method thereof |
| CN113636835B (en) * | 2021-08-30 | 2022-11-18 | 武汉理工大学 | Anorthite heat storage ceramic prepared from magnesium slag and preparation method thereof |
| CN114920578A (en) * | 2022-07-20 | 2022-08-19 | 淄博金狮王科技陶瓷集团有限公司 | Preparation method of porous anorthite/gehlenite complex-phase ceramic with low sintering shrinkage |
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