CN103951446A - Method for preparing beta-SiAlON multiphase material by using ceramic polishing waste residue and coal gangue - Google Patents
Method for preparing beta-SiAlON multiphase material by using ceramic polishing waste residue and coal gangue Download PDFInfo
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- waste residue
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Abstract
The invention relates to a method for preparing a beta-SiAlON multiphase material by using ceramic polishing waste residue and coal gangue. The method comprises the following steps: 1) respectively crushing the ceramic polishing waste residue and coal gangue, and then mixing ceramic polishing waste residue fine powder, coal gangue fine powder and fine carbon powder at a mass ratio of 1:(5-15):(1-5) to obtain a mixture; 2) adding absolute ethyl alcohol into the mixture, performing wet grinding, then drying, adding a binding agent, uniformly mixing, performing pre-press molding under the pressure of 50-100Mpa, then sintering at 1450-1600 DEG C under a nitrogen atmosphere, cooling, and obtaining the beta-SiAlON multiphase material after cooling to the room temperature. According to the method disclosed by the invention, a beta-SiAlON refractory material is prepared by using the ceramic polishing waste residue and coal gangue, so that the environmental protection requirements of performing harmless, yield-reducing and resourceful treatment on solid waste can be achieved, and the additional values of such resources can be improved; the method has good social and economic benefits.
Description
Technical field
The present invention relates to field prepared by industrial solid castoff resource circulation utilization and novel refractory, be specially a kind of method of utilizing ceramic polished waste residue and coal gangue to prepare β-SiAlON composite diphase material.
Background technology
β-SiAlON is β-Si
3n
4with AlN, Al
20
3sosoloid, form available Si
6-zal
zo
zn
8-zrepresent, wherein z represents that Al replaces the atom number of Si.In the time of 1750 ℃, Si
6-zal
zo
zn
8-zcompositional range is from z=0 to z=4.2.The character of β-SiAlON is relevant with z value, and with the increase of z value, unit cell dimension increases, and causes key to weaken by force, short texture, thus the density of making, Young's modulus, folding strength, thermal expansivity decline.β-SiAlON phase crystal grain is long column shape conventionally in addition, in various single-phase SiAlON, has the highest Room-Temperature Fracture Toughness.And the thermal expansivity (2.7 * 10 of β-SiAlON
-6℃
-1) than β-Si
3n
4(3.5 * 10
-6℃
-1) little, so β-SiAlON has than β-Si
3n
4more excellent heat-shock resistance.The oxidation-resistance of β-SiAlON is obviously better than Si simultaneously
3n
4and it is close with SiC.β-SiAlON and molten metal have good consistency, have the ability of very high anti-molten metal attack.
The main synthetic method of β-SiAlON can be divided into high-temperature solid phase reaction method, self propagating high temperature (SHS) synthesis method (combustion method), metallic reducing nitriding, carbothermal reduction-nitridation synthesis method (CRN).
(1) high-temperature solid phase reaction method:
To Si
3n
4in powder, interpolation waits AlN and the Al of mole number
2o
3, and at high temperature AlN and Al
2o
3be solidly soluted into β-Si
3n
4in go, the raw material of different proportionings can obtain β-SiAlON that z value is different, its building-up reactions formula is:
(6-z)Si
3N
4+zAlN+zAl
2O
3=3Si
6-zAl
zO
zN
8-z
(2) self-propagating reaction synthesis method
With Si powder, AlN and α-Si
3n
4for raw material, with heating element, light the titanium particle on reaction mixture top, and produce 2000 ℃ of above high temperature, make reaction mixture take fire (nitrogenizing reaction).Because this combustion reactions has very strong exothermic effect, once after lighting, just can spontaneously maintain, and with the form of combustion wave with 2mms
-1speed spread forward, therefore within several minutes, just complete the synthetic of β-SiAlON.The chemical formula of this combustion synthesis reaction can be expressed as:
Si+Si
3N
4+SiO
2+AlN+N
2(g)→Si
6-zAl
zO
zN
8-z
Whole nitridation process completed in several minutes, and the z value of β-SiAlON that SHS method is synthetic is restricted, and is generally 0.3-0.6.
(3) metallic reducing nitriding
For reducing costs, actual industrialization adopts more in producing be that metallic reducing nitrogenize mode is prepared β-SiAlON, in alumina raw material, and by adding the method for Pure Silicon Metal and aluminium powder, under nitrogen protection, direct synthetic β-SiAlON phase.Its reaction equation is:
(6-z)Si+z/3Al+z/3Al
2O
3+(4-0.5z)N
2=Si
6-zAl
zO
zN
8-z
(4) carbothermal reduction-nitridation synthesis method
Before three kinds of methods due to the expensive (Si of raw material
3n
4, AlN, Al
2o
3or silica flour,
Aluminium powder), energy consumption requires harshness to limit it in industrial scale operation greatly and to equipment and complete processing.Carbothermal reduction-nitridation becomes the emphasis of research due to its economic feasibility.
(6-z)SiO
2+0.5zAl
2O
3+(4-0.5z)N
2+(12-1.5z)C=Si
6-zAl
zO
zN
8-z+(12-1.5z)CO
Carbothermal reduction-nitridation is mainly to be rich in SiO
2, Al
2o
3material be raw material, add appropriate carbon dust as reductive agent, synthetic β-SiAlON under nitrogen atmosphere.
Ceramic polished waste residue, along with the fast development of ceramic industry, ceramic industry waste material waste residue is increasing, not only urban environment is exerted heavy pressures on, but also limited the development of urban economy and the Sustainable development of ceramic industry, so the processing of ceramic industry waste material waste residue with utilize extremely important.Grinding and polishing operation will, from adobe (porcelain brick) surface removal 0.5-0.7 millimeter upper layer, be produced 1 square metre of polished tile and will form the waste residues of polished tiles of 2.1 kilograms of left and right conventionally.
At present, the processing of China's ceramic industry waste material waste residue with utilize degree lower, existing treatment process has filling filtrate (CN1636887A) that the embrane method done processes, produces ultra-thin ceramic polished tile that (CN1683282A, carries out ultra micro thinning processing to ceramic polished waste residue or ceramic waste material and ceramic polished brick batching, powder after dry ultra micro refinement, to after dried pressed by powder moulding, burn till, polishing obtains finished product), foamed ceramics powder (CN102200354A), light ceramic material (CN1463947A, by ceramic polished waste residue, pottery clay, high temperature sand and hypothermia grait form), ceramic tile blank (CN102617123A, 18～40 parts, porcelain sand, 20～30 parts of clays, 1～10 part of limestone particle, 3～15 parts of wollastonite grains, 3～10 parts of ornamental brick sludge silts, 15～45 parts, ceramic polished waste residue, 1～2 part of water glass, 0.15～0.4 part of thinner, 0.05～0.2 part of tripoly phosphate sodium STPP, appropriate water), most landfill methods that adopt are processed, cause a large amount of waste residues to tie up arable land, make water and air be subject to severe contamination.Therefore,
How high efficiente callback utilizes ceramic polished waste residue, promotes the primary study content that added value has become Sustainable Socioeconomic Development and industrial solid castoff resource circulation utilization.
Coal gangue is the barren rock of coal association, is a kind of of mining industry solid waste.The discharge refuse amount of coal gangue accounts for 10%～25% of coal mining amount at present, has become China's accumulative total volume of cargo in storage and the maximum waste of occupied ground.Coal gangue is mainly by SiO
2, Al
2o
3and Fe
2o
3form, account for the more than 80% of total content, there is certain calorific value.Wherein available mineral are mainly SiO
2, Al
2o
3, C, Fe
2o
3, FeS
2and the compound that contains the elements such as Ca, Na, K.
Coal gangue, as waste, also can cause detrimentally affect to environment.Specifically have: one, affect the utilization of land resources, a large amount of coal gangues of stacking take a large amount of land resources on the one hand, also make on the other hand surrounding ground barren and be difficult to utilize, thereby impact is than stacking the larger land resources of area; Two, atmospheric pollution.The long-term coal gangue of stacking can be oxidized in air, even can spontaneous combustion when serious, thus can discharge SO
2, H
2the obnoxious flavoures such as S, pollute air.Three, water and soil pollutes.Coal gangue is subject to the impact of rainfall or for a long time in impregnation state, can make objectionable constituent wherein enter around in water body or soil, finally endangers whole ecotope and human health.Four, landslide and rubble flow.Once coal gangue hill is piled up too high, the gradient is excessive, is easy to form landslide, when the effects such as rainfall make the water content of coal gangue hill reach capacity state, rubble flow probably occurs.
Coal gangue, as potential resources, has the several functions attributes such as clay, rock, coal, industrial chemicals, element resource storehouse, inert material concurrently, has comprehensive Utilization Ways widely.The at present domestic utilization to coal gangue, focuses mostly in traditional field such as building materials, masonries, and added value of product is not high, and it is quite large to be subject to the impact of transportation radius.The comprehensive platform of China < < coal gangue utilizes technical policy will put > > and points out, coal gangue comprehensive utilization is to be utilized as in a large number emphasis, utilize in a large number coal gangue technology as main direction coal gangue power generation, coal gangue building materials and goods, reclaim backfill and coal gangue hill harmless treatment etc., the Technology of Comprehensive Utilization of Coal Gangue of develop high-tech content, high added value and product.
The report that existing ceramic polished waste residue or coal gangue are prepared refractory materials has:
CN200910076061.5(publication number is CN101456738A) a kind of synthetic method of magnesium A Long/β-composite ceramics material is disclosed, belong to structural ceramics and technical field of refractory materials.In synthesis material proportioning of the present invention, the percentage composition of coal gangue is 1～40%, with the percentage composition of tail skid brick powder, is 45～90%, with the percentage composition of rear magnesia carbon brick powder, is 5～15%, and the add-on of carbon is 2～12%.After mixing match raw material, under logical nitrogen atmosphere, heat-treat synthetic, synthesis temperature is 1500～1850 ℃, and soaking time is 1-10h, and nitrogen pressure is between 0.1-20MPa, the percentage composition that in synthetic composite diphase material, the percentage composition of magnesium A Long is 65～95%, β-Sai Long is 5～35%.In this invention raw material, owing to containing a large amount of MgO in magnesia carbon brick, therefore can only produce magnesium A Long/composite ceramics, in product, β-SiAlON thing is mutually impure.
At present, not yet retrieve the report that uses coal gangue, ceramic polished slag to prepare β-SiAlON composite diphase material.
Summary of the invention
The object of the invention is is to utilize the present situations such as insufficient, contaminate environment for ceramic polished waste residue and coal gangue, spy provides a kind of it has been combined to the technical scheme of utilization, significant for the added value of the ceramic polished waste residue of increase and coal gangue and the mode of developing industrial solid castoff utilization.
A kind of method of utilizing ceramic polished waste residue and coal gangue to prepare β-SiAlON composite diphase material provided by the invention, the method comprises the following steps:
1) ceramic polished waste residue and coal gangue are crushed to respectively to granularity and are less than or equal to 48 μ m, then by ceramic polished waste residue fine powder, coal gangue fine powder and carbon dust fine powder 1:(5～15 in mass ratio): the ratio of (1～5) is mixed, and obtains compound;
2) compound is added to dehydrated alcohol wet-milling, wet-milling 6-10 hour, then 100～120 ℃ of oven dry, add caking agent, after mixing under the pressure of 50～100Mpa pre-molding, then 1450～1600 ℃ of sintering 4～6 hours under nitrogen atmosphere, stop passing into nitrogen after being cooled to 800 ℃, obtain β-SiAlON composite diphase material after being cooled to room temperature.
Wherein:
Described ceramic polished waste residue is the 0.5-0.7 millimeter upper layer from the adobe surface removal of porcelain brick; The composition that it contains following mass percent: Al
2o
315%～20%, basic oxide CaO, MgO and K/Na compound total content 7%～15%, SiO
2content 65%～75%;
Described coal gangue, the composition that contains following mass percent: SiO
2(containing SiC) 50%～70%, Al
2o
320%～45%, C5%～15%;
Described carbon dust is Graphite Powder 99, coke powder, activity charcoal powder, wood charcoal powder or carbon black etc., and its mass percent is more than or equal to 99.5%.
During described wet-milling, every 100g compound adds 5～10ml dehydrated alcohol.
Described caking agent is organic caking agent nontoxic and that can volatilize under more than 500 ℃ high temperature, as polyvinyl alcohol or Xylo-Mucine etc.
Caking agent need to be mixed with the aqueous solution while using, and its mass concentration is 3～5%, and addition is to add 0.08～0.12ml in every g compound.
Wherein, logical nitrogen gas concn is more than or equal to 99.5%.
Preferably, method provided by the invention comprises the following steps:
1) ceramic polished waste residue, coal gangue are pulverized respectively, crossed 45 μ m sieves;
2) by the ratio mixing of 1:7:2 in mass ratio of ceramic polished waste residue fine powder, coal gangue fine powder and activity charcoal powder, obtain compound;
3) compound is added to dehydrated alcohol wet-milling 4 hours, every 100g compound adds 5-10ml dehydrated alcohol, then 100 ℃ are dried 6 hours, the polyvinyl alcohol water solution that interpolation mass concentration is 4%, and addition is that every 10g adds 1.0ml, after mixing under 80MPa pressure pre-molding, then the logical lower 1500 ℃ of sintering 6h of nitrogen condition continue to pass into nitrogen to be cooled to 800 ℃ with stove after sintering, stop logical nitrogen, cool to room temperature, obtains β-SiAlON composite diphase material.
The advantage of preparation β-SiAlON material provided by the invention:
1, the present invention proposes a kind of mode of utilizing of simultaneously utilizing ceramic polished waste residue and coal gangue two large industrial solid castoffs, adopt carbothermal reduction-nitridation method sintering to prepare high performance β-SiAlON multiple phase refractory material.
The present invention takes full advantage of the residual carbon in coal gangue, provides carbon source on the one hand, has saved on the other hand energy;
Be different from single coal gangue and prepare SiAlON, the SiC containing in ceramic polished waste residue both can serve as reductive agent in reaction, improved β-SiAlON synthetic ratio, also can be used as crystal whisker materials simultaneously, reached complex phase toughness reinforcing, improved the physicals of material.
2, the medium that the present invention uses in wet-milling process is dehydrated alcohol, object is to prevent that calcium salt too much in ceramic polished waste residue, magnesium salts from reacting formation block insolubles (calcium hydroxide, magnesium hydroxide etc.) with water, generate precipitation (calcium carbonate, magnesiumcarbonate etc.) with salt of weak acid simultaneously
Be unfavorable for the mass transfer diffusion of sintering experiment.
3, the present invention utilizes ceramic polished waste residue and coal gangue to prepare β-SiAlON refractory materials, not only reached the environmental requirement of, minimizing innoxious to solid waste, recycling treatment, and improved the added value of such resource, there is good Social benefit and economic benefit.
4, prior art as CN200910180637.2(publication number be CN101671198A) to disclose a kind of be to using coal gangue and waste refractory materials (waste magnesia carbon bricks, waste sliding brick) and wood-dust pore forming agent as raw material, according to quality than coal gangue 35～55%, with rear magnesia carbon brick 3～10%, mix with tail skid brick 10～50%, wood chip 5～40%, after moulding in air atmosphere, at 1340 ℃～1460 ℃ temperature, be incubated 2-6h, obtain synthetic sintered blank.Although this invention belongs to preparation β-SiAlON material, raw material and technique are all different.Main difference part is: 1) raw material of the present invention is used solid waste, greatly saves existing Mineral resources (andaluzite, clay, kaolinite etc.); 2) process optimization.The strict proportioning raw materials of calculating, without burying carbon, does not have after baking except the technique of surplus carbon, saves the energy.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the inventive method.
Fig. 2 is the SEM micro-structure diagram of β-SiAlON crystalline phase of β-SiAlON material of preparing of the embodiment of the present invention.
Fig. 3 is the SEM micro-structure diagram of the SiC whisker of β-SiAlON material of preparing of the embodiment of the present invention.
Fig. 4 is β-SiAlON XRD(2 θ angle that the embodiment of the present invention prepares) actual measurement peak (on) and standard card (under, XRD standard card (00-048-1616)) comparison.
Embodiment
Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
Utilize shanxi coal spoil and Foshan Ceramic polishing slag to prepare β-SiAlON material.By X-ray fluorescence spectra analysis (XRF), obtain the chemical constitution of coal gangue and ceramic polished waste residue, in Table 1.
Table 1: the chemical composition (mass percent: %) in coal gangue and ceramic polished waste residue
| Raw material | SiO 2 | Al 2O 3 | C | CaO | Fe 2O 3 | MgO | K 2O |
| Coal gangue fine powder | 50.50 | 43.16 | 13.64 | 1.49 | 1.57 | 0.8 | 0.8 |
| Ceramic polished waste residue | 67.99 | 19.64 | / | 1.68 | 0.47 | 3.36 | 1.68 |
The z value that design generates β-SiAlON is 3, i.e. the mol ratio 1:1 of Si, Al element in raw material, specifically preparation method's following (particular flow sheet is shown in Fig. 1):
1, ceramic polished waste residue, coal gangue are pulverized respectively, crossed 45 μ m sieves, granularity is as shown in table 2:
Table 2: coal gangue and ceramic polished waste residue granularity
| Raw material | Purity granularity | Raw material sources |
| Coal gangue fine powder | /45μm | Shanxi |
| Ceramic polished waste residue | /45μm | Foshan |
| Activity charcoal powder | 99.55μm | —— |
2, by the ratio mixing of 1:7:2 in mass ratio of ceramic polished waste residue fine powder, coal gangue fine powder and activity charcoal powder, obtain compound;
3, compound is added to dehydrated alcohol wet-milling 4 hours, every 100g compound adds 5-10ml dehydrated alcohol, and then 100 ℃ are dried 6 hours, the polyvinyl alcohol water solution that interpolation mass concentration is 4%, addition is that every 10g adds 1.0ml, precompressed under 80MPa pressure after mixing
Moulding, then the logical lower 1500 ℃ of sintering 6hSiAlON of nitrogen (purity 99.9 ℅) condition continue to pass into nitrogen to be cooled to 800 ℃ with stove after sintering, stop logical nitrogen, and cool to room temperature, obtains β-SiAlON composite diphase material.
3, with scanning electron microscopy analysis (SEM, scanning electron microscope) and X-ray diffraction (XRD), β-SiAlON composite diphase material is analyzed, wherein β-SiAlON crystalline phase is shown in Fig. 2, and SiC whisker is shown in Fig. 3, and XRD is shown in Fig. 4, and result shows:
Fig. 2: finding hexagonal columnar crystalline substance is β-SiAlON crystal, and good crystalline phase has been synthesized in this experiment as seen.Due to the complicacy of raw material, inevitably there is a small amount of silicon carbide, Al
2o
3phase, wherein, SiC can be used as the toughness reinforcing whisker of complex phase (Fig. 3), can improve the performance of product.
Fig. 4 is sample XRD figure spectrum, very identical with XRD standard card (00-048-1616, β-SiAlON) peak type, then carries out semi-quantitative analysis discovery, and β-SiAlON principal crystalline phase ratio is about 66.2%, 28.4% SiC.
Conclusion: the present invention uses ceramic polished waste residue, carbon dust and coal gangue successfully to prepare β-SiAlON composite diphase material.
Although, above used general explanation, embodiment and test, the present invention is described in detail, on basis of the present invention, can make some modifications or improvements it, and this will be apparent to those skilled in the art.Therefore, these modifications or improvements, all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (10)
1. utilize ceramic polished waste residue and coal gangue to prepare a method for β-SiAlON composite diphase material, the method comprises the following steps:
1) ceramic polished waste residue and coal gangue are pulverized respectively, then by ceramic polished waste residue fine powder, coal gangue fine powder and carbon dust fine powder 1:(5～15 in mass ratio): the ratio of (1～5) is mixed, and obtains compound;
2) compound is added to dehydrated alcohol wet-milling, then dries, add caking agent, after mixing under the pressure of 50～100Mpa pre-molding, 1450～1600 ℃ of sintering under nitrogen atmosphere then, cooling, obtains β-SiAlON composite diphase material after being cooled to room temperature.
2. method according to claim 1, is characterized in that, the method comprises the following steps:
1) ceramic polished waste residue and coal gangue are crushed to respectively to granularity and are less than or equal to 48 μ m, then by ceramic polished waste residue fine powder, coal gangue fine powder and carbon dust fine powder 1:(5～15 in mass ratio): the ratio of (1～5) is mixed, and obtains compound;
2) compound is added to dehydrated alcohol wet-milling, wet-milling 6-10 hour, then 100～120 ℃ of oven dry, add caking agent, after mixing under the pressure of 50～100Mpa pre-molding, then 1450～1600 ℃ of sintering 4～6 hours under nitrogen atmosphere, stop passing into nitrogen after being cooled to 800 ℃, obtain β-SiAlON composite diphase material after being cooled to room temperature.
3. method according to claim 1, is characterized in that, described ceramic polished waste residue is the 0.5-0.7 millimeter upper layer from the adobe surface removal of porcelain brick.
4. method according to claim 3, is characterized in that, the composition that described ceramic polished waste residue contains following mass percent: Al
2o
315%～20%, basic oxide CaO, MgO and K/Na compound total content 7%～15%, SiO
2(containing SiC) content 65%～75%.
5. method according to claim 1, is characterized in that, described coal gangue, the composition that contains following mass percent: SiO
250%～70%, Al
2o
320%～45%, C5%～15%; Described carbon dust is Graphite Powder 99, coke powder, activity charcoal powder, wood charcoal powder or carbon black.
6. method according to claim 1, is characterized in that, during described wet-milling, every 100g compound adds 5-10ml dehydrated alcohol.
7. method according to claim 1, is characterized in that, described caking agent is organic caking agent nontoxic and that can volatilize under more than 500 ℃ high temperature.
8. method according to claim 1, is characterized in that, binding agent is polyvinyl alcohol or Xylo-Mucine.
9. method according to claim 1, is characterized in that, caking agent need to be mixed with the aqueous solution while using, and its mass concentration is 3～5%, and addition is to add 0.08～0.12ml in every g compound.
10. according to the method described in claim 1-9 any one, it is characterized in that, method provided by the invention comprises the following steps:
1) ceramic polished waste residue, coal gangue are pulverized respectively, crossed 45 μ m sieves;
2) by the ratio mixing of 1:7:2 in mass ratio of ceramic polished waste residue fine powder, coal gangue fine powder and activity charcoal powder, obtain compound;
3) compound is added to dehydrated alcohol wet-milling 4 hours, every 100g compound adds 5-10ml dehydrated alcohol, then 100 ℃ are dried 6 hours, the polyvinyl alcohol water solution that interpolation mass concentration is 4%, and addition is that every 10g adds 1.0ml, after mixing under 80MPa pressure pre-molding, then the logical lower 1500 ℃ of sintering 6h of nitrogen condition continue to pass into nitrogen to be cooled to 800 ℃ with stove after sintering, stop logical nitrogen, cool to room temperature, obtains β-SiAlON composite diphase material.
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| CN107399988A (en) * | 2017-08-22 | 2017-11-28 | 东北大学 | A kind of method for preparing alumina carbon SiClx composite porous ceramic using aluminium silicon systems industrial residue |
| CN109133875A (en) * | 2018-09-14 | 2019-01-04 | 洛阳科创新材料股份有限公司 | A kind of magnesium carbonaceous slide plate and preparation method thereof adding SiALON powder |
| CN114763303A (en) * | 2021-01-13 | 2022-07-19 | 中国科学院过程工程研究所 | Coal gangue-based heating material and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106634557A (en) * | 2016-12-08 | 2017-05-10 | 长兴天晟能源科技有限公司 | High-temperature-resisting and oxidation-resisting coating for SiAlON-AlN-TiN-based stainless steel |
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| CN107399988B (en) * | 2017-08-22 | 2020-10-16 | 东北大学 | Method for preparing alumina-silicon carbide composite porous ceramic by using aluminum-silicon industrial waste residues |
| CN109133875A (en) * | 2018-09-14 | 2019-01-04 | 洛阳科创新材料股份有限公司 | A kind of magnesium carbonaceous slide plate and preparation method thereof adding SiALON powder |
| CN114763303A (en) * | 2021-01-13 | 2022-07-19 | 中国科学院过程工程研究所 | Coal gangue-based heating material and preparation method thereof |
| CN114763303B (en) * | 2021-01-13 | 2023-05-02 | 中国科学院过程工程研究所 | Gangue-based heating material and preparation method thereof |
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| CN103951446B (en) | 2015-08-26 |
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