CN103265304A - Low-temperature synthesized composite ceramic for CFB (Circulating Fluidized Bed) and preparation method of composite ceramic - Google Patents
Low-temperature synthesized composite ceramic for CFB (Circulating Fluidized Bed) and preparation method of composite ceramic Download PDFInfo
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Abstract
The invention belongs to the field of preparation of ceramic and in particular relates to low-temperature synthesized composite ceramic for a CFB (Circulating Fluidized Bed) and a preparation method of the composite ceramic. The composite ceramic is prepared by modifying, stirring, stamping and sintering the following components according to a certain proportion: mullite, silicon carbide, silicon micro powder, Al2O3, SiO2, ZrO2, potassium titanate whisker, silane, titanate, hexadecyl trimethyl ammonium bromide and tabular corundum. According to the low-temperature synthesized composite ceramic for the CFB and the preparation method of the composite material, the formula is reasonable and the preparation process is simple and easy to operate; the toughness and the abrasion resistance of the prepared CFB composite ceramic are greatly improved; and the preparation process adopts low-temperature synthesis, and energy saving and environment friendliness are realized.
Description
Technical field
The invention belongs to ceramic preparation field, relate in particular to the synthetic CFB of a kind of low temperature composite ceramics and preparation method thereof.
Background technology
CFB with its fuel wide accommodation, cheap desulfurization, control pollutant emission, efficiency of combustion height, load regulation rate is big and lime-ash is beneficial to advantages such as comprehensive utilization; become a primary study of clean burning technology, the direction of exploitation; being subjected to various countries' common concern, is a new way that solves save energy and protection environment.But large-scale CFB still has a lot of problems to need to solve in selection, and wherein the wear resistance problem of refractory materials is exactly a great problem.Erosive wear is the problem that various CFB must face with refractory materials, because the characteristic of boiler itself, the refractory materials that is in operation will be subjected to the wearing and tearing of the Solid Bed material of fuel, fuel ash, Wingdale and reaction product thereof every day.
Refractory materials produces and expands or contraction with the lifting of temperature, if this expansion or contraction suffer restraints, material internal can produce stress.Refractory materials is the hard brittle material of heterogeneous body, compare with metal products, because its thermal conductivity and elasticity is less, tensile strength is low, opposing thermal stress damage ability, heat-shock resistance are lower, under the heat shock cycling effect, damaging to whole easily appears earlier ftractureing to peel off eventually in refractory materials, and this is the another major reason that causes the inefficacy of CFB refractory materials.The used lining of anti-material of domestic CFB is as mould material, the combination of prefabricated component is many to be combined into the master with aquation, be aided with the micro mist cohesion, under 900 ℃ working temperature, be difficult to sintering, cause the intensity under its normal temperature not reach design requirements, and under arms under the temperature, intensity descends significantly, cause material property to lose efficacy, moreover mould material also needs strict baking process, and it is consuming time to take a lot of work, and causes that the uncertain human factor that material property descends increases, and the refractory brick through firing more than 1400 ℃, though be ceramic combination, the toughness deficiency, over-all properties can not satisfy the actual demand of CFB working condition.
Summary of the invention
In order to overcome the prior art deficiency, the invention provides good toughness, CFB composite ceramics and preparation method thereof that a kind of low temperature of high abrasion is synthetic.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
The CFB composite ceramics that a kind of low temperature is synthetic is to be made by following quality proportion raw material: mullite 12 ~ 25%, silicon carbide 10-20%, silicon powder 3-5%, Al
2O
36% ~ 10%, SiO
25% ~ 10%, ZrO
23% ~ 5%, potassium titanate crystal whisker 2% ~ 6%, silane 0. 2% ~ 0.5%, titanic acid ester 0.2% ~ 0.5% and cetyl trimethylammonium bromide 0.5% ~ 1.5%, surplus is plate diamond spar.
Preferably, described composite ceramics is made by following quality proportion raw material: diameter is that the sintering of 0.5 ~ 2mm or electrofused mullite particle 10% ~ 15%, diameter are that the fused mullite particle 2% ~ 10% of 0.01-0.05mm, silicon-carbide particle 10% ~ 20%, diameter that diameter is 0.5 ~ 1mm are that silicon powder particle 3% ~ 5%, the diameter of 5-20 μ m is the Al of 30-100nm
2O
3Particle 6% ~ 10%, diameter are the SiO of 10-50nm
2Particle 5% ~ 10%, diameter are the ZrO of 10-100nm
2Particle 3% ~ 5%, potassium titanate crystal whisker 2% ~ 6%, silane 0.2% ~ 0. 5%, titanic acid ester 0.2% ~ 0.5%, cetyl trimethylammonium bromide 0.5% ~ 1.5%, diameter are the plate diamond spar particle 10% ~ 20% of 0.01-0.1mm, and surplus is that diameter is the plate diamond spar particle of 1 ~ 5mm.
The synthetic CFB of the described a kind of low temperature preparation method of composite ceramics, step is as follows:
The first step: get each component raw material according to the quality proportioning, and respectively with Al
2O
3, SiO
2Mix with cetyl trimethylammonium bromide and to carry out surface modification, with ZrO
2Carry out surface modification with silane mixture, the whisker potassium titanate is mixed with titanic acid ester, carry out surface modification;
Second step: the mixing of the first step products therefrom is mixed with remaining component raw material, stir into the fluidised form colloidal mixture, then this mixture is positioned in the mould, pressurization and vibration, make base substrate, make base substrate weather aging to intensity be 〉=1 Mpa, then base substrate is separated with mould;
The 3rd step: the second step gained base substrate is heat-treated: be warming up to 600 ℃ with 2 ~ 5 ℃/minute and also be incubated, cool off then, namely obtain final finished and namely get the synthetic CFB composite ceramics of a kind of low temperature.
Preferably, described preparation method in the first step, uses nano-dispersed equipment, the mixture that needs surface modification is carried out 30-50 minute dispersion.
Preferably, described preparation method, in the first step, the time of described dispersion is 40 minutes.
Preferably, described preparation method in second step, uses shear mixer mixture to all components under normal temperature, normal pressure to stir, and the time is 20-40 minute.
Preferably, described preparation method, in second step, the vibrational frequency of pressurization and vibration is 60 times
/Minute, amplitude is 1mm, pressure is 5Mpa.
Preferably, described preparation method, in the 3rd step, heat-up rate is 4 ℃/minute, is 24 hours at 600 ℃ insulation durations.
Utilize nano level Al
2O
3, SiO
2And ZrO
2Small-size effect and surface and interfacial effect because of its nano material, and the strengthening and toughening mechanism of potassium titanate crystal whisker, by pressing reasonable combinations of particle sizes with the matrix major ingredient after the modification, and adopt colloidal state consolidation in-situ forming and thermal treatment process to control, realized in the goods with inorganic polymer and whisker, needle-like mullite crystallite constitutes the space framework, fire-resistant, wear-resisting synthetic material is fine and close fills, the novel microstructure of nanoparticle even dispersion, and in making up between each thing phase component with covalent linkage (or ionic linkage) bonding, thereby guaranteed mechanical behavior under high temperature and the Themal stress damage resistance property of member excellence.Compare with the used lining material of existing CFB, intensity has improved 50 ~ 80%, and service life of equipment was extended to more than 25,000 hours by several thousand hours.
The CFB that the present invention prepares is as follows with the performance of composite ceramics:
Cold crushing strength 〉=150 Mpa; Strength at normal temperature 〉=20 Mpa; Mohs' hardness 〉=8; Volume density 〉=2.80 g/cm
3Void content≤5%; Thermal shock resistance (1100 ℃ of water-cooleds) 〉=60 times; Linear expansivity :+0.2%.
The present invention compared with prior art has following advantage:
1) prescription is reasonable, and preparation technology is simple to operation, and the CFB for preparing improves greatly with composite ceramics toughness, wear resistance;
2) preparation technology uses low temperature synthetic, energy-conserving and environment-protective.
Embodiment
The present invention will be further described below in conjunction with specific embodiment.
Embodiment 1
Cut-off is that the fused mullite particle 2% of 0.01mm, silicon-carbide particle 10%, diameter that diameter is 0.5mm are that silicon powder particle 3%, the diameter of 5 μ m is the Al of 30nm for the electrofused mullite particle 10% of 0.5mm, diameter directly
2O
3Particle 6%, diameter are 10 SiO
2Particle 5 %, diameter are the ZrO of 10nm
2Particle 3 %, potassium titanate crystal whisker 2%, silane 0.2%, titanic acid ester 0.2%, cetyl trimethylammonium bromide 0.5%, diameter are the plate diamond spar particle 10% of 0.01mm, and surplus is that diameter is the plate diamond spar of 1mm.
The first step: get each component raw material according to the quality proportioning, and respectively with Al
2O
3, SiO
2Mix with cetyl trimethylammonium bromide, with ZrO
2With silane mixture, the whisker potassium titanate is mixed with titanic acid ester, three kinds of mixtures are used nano-dispersed equipment respectively, carry out 30 minutes dispersion, carry out surface modification;
Second step: the mixing of the first step products therefrom is mixed with remaining component raw material, and use shear mixer under normal temperature, normal pressure, above-mentioned mixed mixture to be stirred, the time is 20 minutes, is stirred to the fluidised form colloidal mixture, then this mixture is positioned in the mould, with 60 times
/Minute vibrational frequency, amplitude 1mm, pressure are under the requirement of 5Mpa, the mixture pressurization and vibration in the mould makes base substrate, treat the base substrate weather aging to intensity for behind 〉=1 Mpa, base substrate is separated with mould;
The 3rd step: the second step gained base substrate is heat-treated: be warming up to 600 ℃ and be incubated 24 hours with 2 ℃/minute, cool off then, namely obtain final finished and namely get the synthetic CFB composite ceramics of a kind of low temperature.
The CFB of present embodiment preparation with the principal character physical and chemical index of composite ceramics is:
Cold crushing strength: 160Mpa
Mohs' hardness: 9
Thermal shock resistance (100 ℃ of water-cooleds) 67 times
Strength at normal temperature: 22Mpa
The CFB of present embodiment preparation is really outstanding at CFB burner hearth emulsion zone Use Limitation with composite ceramics.
Embodiment 2
Cut-off is that the fused mullite particle 10% of 0.05mm, silicon-carbide particle 20%, diameter that diameter is 1mm are that silicon powder particle 5%, the diameter of 20 μ m is the Al of 100nm for the fused mullite particle 15% of 2mm, diameter directly
2O
3Particle 10%, diameter are the SiO of 50nm
2Particle 10%, diameter are the ZrO of 100nm
2Particle 5%, potassium titanate crystal whisker 6%, silane 0.5%, titanic acid ester 0.5%, cetyl trimethylammonium bromide 1.5%, diameter are the plate diamond spar particle 15% of 0.1mm, and surplus is that diameter is the plate diamond spar of 5mm.
The first step: get each component raw material according to the quality proportioning, and respectively with Al
2O
3, SiO
2Mix with cetyl trimethylammonium bromide, with ZrO
2With silane mixture, the whisker potassium titanate is mixed with titanic acid ester, three kinds of mixtures are used nano-dispersed equipment respectively, carry out 50 minutes dispersion, carry out surface modification;
Second step: the mixing of the first step products therefrom is mixed with remaining component raw material, and use shear mixer under normal temperature, normal pressure, above-mentioned mixed mixture to be stirred, the time is 40 minutes, is stirred to the fluidised form colloidal mixture, then this mixture is positioned in the mould, with 60 times
/Minute vibrational frequency, amplitude 1mm, pressure are under the requirement of 5Mpa, the mixture pressurization and vibration in the mould makes base substrate, treat the base substrate weather aging to intensity for behind 〉=1 Mpa, base substrate is separated with mould;
The 3rd step: the second step gained base substrate is heat-treated: be warming up to 600 ℃ and be incubated 24 hours with 5 ℃/minute, cool off then, namely obtain final finished and namely get the synthetic CFB composite ceramics of a kind of low temperature.
The CFB of present embodiment preparation with the principal character physical and chemical index of composite ceramics is:
Normal temperature is withstand voltage: 158Mpa
The anti-folding of normal temperature: 26Mpa
Thermal shock resistance (100 ℃ of water-cooleds): 92 times
Mohs' hardness: 9
The CFB of present embodiment preparation is really outstanding at CFB burner hearth emulsion zone Use Limitation with composite ceramics.
Embodiment 3
Cut-off is that the fused mullite particle 6% of 0.03mm, silicon-carbide particle 15%, diameter that diameter is 0.8mm are that silicon powder particle 4%, the diameter of 13 μ m is the Al of 70nm for the sintering of 1.3mm or electrofused mullite particle 13%, diameter directly
2O
3Particle 8%, diameter are the SiO of 30nm
2Particle 7%, diameter are the ZrO of 60nm
2Particle 4%, potassium titanate crystal whisker 4%, silane 0.3%, titanic acid ester 0.3%, cetyl trimethylammonium bromide 0.9%, diameter are the plate diamond spar particle 15% of 0.07mm, and surplus is that diameter is the plate diamond spar of 3mm.
The first step: get each component raw material according to the quality proportioning, and respectively with Al
2O
3, SiO
2Mix with cetyl trimethylammonium bromide, with ZrO
2With silane mixture, the whisker potassium titanate is mixed with titanic acid ester, three kinds of mixtures are used nano-dispersed equipment respectively, carry out 40 minutes dispersion, carry out surface modification;
Second step: the mixing of the first step products therefrom is mixed with remaining component raw material, and use shear mixer under normal temperature, normal pressure, above-mentioned mixed mixture to be stirred, the time is 30 minutes, is stirred to the fluidised form colloidal mixture, then this mixture is positioned in the mould, with 60 times
/Minute vibrational frequency, amplitude 1mm, pressure are under the requirement of 5Mpa, the mixture pressurization and vibration in the mould makes base substrate, treat the base substrate weather aging to intensity for behind 〉=1 Mpa, base substrate is separated with mould;
The 3rd step: the second step gained base substrate is heat-treated: be warming up to 600 ℃ and be incubated 24 hours with 3 ℃/minute, cool off then, namely obtain final finished and namely get the synthetic CFB composite ceramics of a kind of low temperature.
Claims (8)
1. the CFB composite ceramics that low temperature is synthetic is characterized in that, is to be made by following quality proportion raw material: mullite 12 ~ 25%, silicon carbide 10-20%, silicon powder 3-5%, Al
2O
36% ~ 10%, SiO
25% ~ 10%, ZrO
23% ~ 5%, potassium titanate crystal whisker 2% ~ 6%, silane 0. 2% ~ 0.5%, titanic acid ester 0.2% ~ 0.5% and cetyl trimethylammonium bromide 0.5% ~ 1.5%, surplus is plate diamond spar.
2. the synthetic CFB composite ceramics of a kind of low temperature as claimed in claim 1, it is characterized in that, made by following quality proportion raw material: diameter is that the sintering of 0.5 ~ 2mm or electrofused mullite particle 10% ~ 15%, diameter are that the fused mullite particle 2% ~ 10% of 0.01-0.05mm, silicon-carbide particle 10% ~ 20%, diameter that diameter is 0.5 ~ 1mm are that silicon powder particle 3% ~ 5%, the diameter of 5-20 μ m is the Al of 30-100nm
2O
3Particle 6% ~ 10%, diameter are the SiO of 10-50nm
2Particle 5% ~ 10%, diameter are the ZrO of 10-100nm
2Particle 3% ~ 5%, potassium titanate crystal whisker 2% ~ 6%, silane 0.2% ~ 0. 5%, titanic acid ester 0.2% ~ 0.5%, cetyl trimethylammonium bromide 0.5% ~ 1.5%, diameter are the plate diamond spar particle 10% ~ 20% of 0.01-0.1mm, and surplus is that diameter is the plate diamond spar particle of 1 ~ 5mm.
3. use the preparation of composite ceramics as the synthetic CFB of the arbitrary described a kind of low temperature of claim 1-2
Method is characterized in that, step is as follows:
The first step: get each component raw material according to the quality proportioning, and respectively with Al
2O
3, SiO
2Mix with cetyl trimethylammonium bromide and to carry out surface modification, with ZrO
2Carry out surface modification with silane mixture, the whisker potassium titanate is mixed with titanic acid ester, carry out surface modification;
Second step: the mixing of the first step products therefrom is mixed with remaining component raw material, stir into the fluidised form colloidal mixture, then this mixture is positioned in the mould, pressurization and vibration, make base substrate, make base substrate weather aging to intensity be 〉=1 Mpa, then base substrate is separated with mould;
The 3rd step: the second step gained base substrate is heat-treated: be warming up to 600 ℃ with 2 ~ 5 ℃/minute and also be incubated, cool off then, namely obtain final finished and namely get the synthetic CFB composite ceramics of a kind of low temperature.
4. the synthetic CFB of a kind of low temperature as claimed in claim 3 preparation method of composite ceramics is characterized in that: in the first step, use nano-dispersed equipment, the mixture that needs surface modification is carried out 30-50 minute dispersion.
5. the synthetic CFB of a kind of low temperature as claimed in claim 4 is with the preparation method of composite ceramics, and it is characterized in that: the time of described dispersion is 40 minutes.
6. the synthetic CFB of a kind of low temperature as claimed in claim 3 is with the preparation method of composite ceramics, and it is characterized in that: in second step, use shear mixer mixture to all components under normal temperature, normal pressure to stir, the time is 20-40 minute.
7. the synthetic CFB of a kind of low temperature as claimed in claim 3 is with the preparation method of composite ceramics, and it is characterized in that: in second step, the vibrational frequency of pressurization and vibration is 60 times
/Minute, amplitude is 1mm, pressure is 5Mpa.
8. the synthetic CFB of a kind of low temperature as claimed in claim 3 is with the preparation method of composite ceramics, and it is characterized in that: in the 3rd step, heat-up rate is 4 ℃/minute, is 24 hours at 600 ℃ insulation durations.
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| CN103588474A (en) * | 2013-11-15 | 2014-02-19 | 哈尔滨工业大学 | Preparation method of magneto-electricity composite ceramic with coating structure |
| CN106083118A (en) * | 2016-06-13 | 2016-11-09 | 孟红琳 | A kind of kiln composite block insulation material of silicon nitride combined silicon carbide and preparation method thereof |
| CN107840668A (en) * | 2017-10-29 | 2018-03-27 | 贵州喜文化艺术有限责任公司 | A kind of ceramic composition and preparation method thereof |
| CN107954733A (en) * | 2017-12-18 | 2018-04-24 | 江南大学 | A kind of original position aluminium borate whisker enhancing CFB boiler high-strength abrasion-proof is moldable |
| CN107954734A (en) * | 2017-12-11 | 2018-04-24 | 蒙娜丽莎集团股份有限公司 | A kind of particle enhancing ceramic thin plate and preparation method thereof |
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| CN103588474A (en) * | 2013-11-15 | 2014-02-19 | 哈尔滨工业大学 | Preparation method of magneto-electricity composite ceramic with coating structure |
| CN106083118A (en) * | 2016-06-13 | 2016-11-09 | 孟红琳 | A kind of kiln composite block insulation material of silicon nitride combined silicon carbide and preparation method thereof |
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| CN113636832A (en) * | 2021-08-20 | 2021-11-12 | 瑞泰科技股份有限公司 | Aluminum zirconium silicon carbide brick for CFB boiler cyclone separator target area and preparation method thereof |
| CN116217250A (en) * | 2023-02-14 | 2023-06-06 | 湖南金铠新材料科技股份有限公司 | Casket-like bowl for sintering whisker reinforced lithium ion battery anode material and preparation method thereof |
| CN116217250B (en) * | 2023-02-14 | 2023-12-12 | 湖南金铠新材料科技股份有限公司 | Casket-like bowl for sintering whisker reinforced lithium ion battery anode material and preparation method thereof |
| CN117567144A (en) * | 2024-01-15 | 2024-02-20 | 山东新广恒节能科技有限公司 | Preparation method of light high-alumina light-weight brick |
| CN117567144B (en) * | 2024-01-15 | 2024-03-19 | 山东新广恒节能科技有限公司 | Preparation method of light high-alumina light-weight brick |
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