CN107299254A - A kind of high-temperature dusty gas separation membrane-porous material and preparation method thereof - Google Patents
A kind of high-temperature dusty gas separation membrane-porous material and preparation method thereof Download PDFInfo
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- CN107299254A CN107299254A CN201710451216.3A CN201710451216A CN107299254A CN 107299254 A CN107299254 A CN 107299254A CN 201710451216 A CN201710451216 A CN 201710451216A CN 107299254 A CN107299254 A CN 107299254A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
- B01D39/2027—Metallic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0001—Making filtering elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/11—Making porous workpieces or articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
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Abstract
The invention discloses the preparation method that a kind of high-temperature dusty gas separates porous Ni-base alloy material.The preparation method of the present invention is mainly,（1）Powder is compounded：High-purity N i, Cr, Al, Y element powder that mass percent is respectively 53 79.5,15 25,5 20 and 0.5 2 are sufficiently mixed；（2）Cold moudling：Mixed powder is granulated, dried, through cold moudling green compact；（3）Green compact are carried out to four stage sintering in vacuum sintering furnace.The present invention reacts synthetically prepared Ni Cr Al Y porous alloys using element powders vacuum-sintering, and internal void is abundant uniform, and open porosity is high, filter efficiency is high, and with excellent high temperature resistant, anti-oxidant, anti-thermal shock and decay resistance, it is high mechanical strength, solderable, it is easy to process.The present invention effectively extends the service life of filter element while raising filtering accuracy and guarantee filtering stability.
Description
Technical field
The present invention relates to a kind of preparation method of porous material, and in particular to is reacted and synthesized by element powders vacuum-sintering
A kind of high-temperature dusty gas separates the preparation method of porous Ni-base alloy material, belongs to air contaminant treatment dedusting technology field.
Background technology
Hot gas filtration technology can improve energy farthest using the physical sensible heat of gas, potential chemical heat
Source utilization rate, process simplification saves equipment investment；Meanwhile, it also avoid carrying out flue gas cooling treatment and wet method removed again
The secondarily polluted water that dirt is brought.Therefore, rationally there is very huge economic value and social benefit using the technology.High temperature
Filter realizes the circular regeneration of filter element typically by the way of pulse backblowing deashing, it is necessary to meet following three aspect
Performance requirement：（1）Good thermal shock resistance and mechanical strength.Temperature during reverse gas cleaning due to purge gas will be less than filtering
The temperature of gas, the stress that filter bears rapid heating and cooling and produced, therefore require that there is excellent thermal shock resistance and mechanical strength.
（2）Filterability is good.The pressure drop of filter depends primarily on the pressure drop of chimney filter, therefore requires that chimney filter has good filterability.
（3）Good high temperature resistant and decay resistance.Filter it is general in high temperature (800-1100 DEG C), it is high pressure (1.0-3.0MPa), strong
Acid, containing long-term work under the environment such as steam, oxygen-containing, its working condition is very severe, therefore requires with excellent high temperature resistant and resistance to
Corrosive nature.The characteristics of sack cleaner is because of its high-effective dust-removing and turn into most widely used filter collector.Such as patent of invention
CN105080222A discloses a kind of pre- dedusting heat sink of sack cleaner, and the device is in pre-duster box house provided with drop
Warm water tube, greatly reduces the temperature of flue gas, reduces big dust particle or stone enters sack cleaner, to a certain extent
Extend the useful life of cloth bag.However, because the cloth bag such as terylene, fiber material is easily sent out in the dusty gas of severe corrosive
The phenomenons such as heat contracting, degraded, oxidation, cause the reduction of filtering accuracy and reduce its service life.With the development of industrial technology,
Gas filtration dedusting technology faces higher operating temperature, stronger corrosive medium, the faster rate of filtration and Geng Gao filtering
Efficiency, and on the market filter have that high temperature oxidation resistance is poor, decay resistance not enough, switching performance is poor mostly,
The high-temperature filter of thermal shock resistance difference or the low problem of mechanical strength, a kind of high filtering precision of exploitation and service life length has very much must
Will.
High-temperature filter is acknowledged as a kind of most potential new dust removal technology for high-temperature flue gas.High temperature filter material mainly has many
Mesoporous metal and the class rigid filtration material of micropore ceramics two.Patent of invention CN102895809A disclose a kind of ceramic filtering device and
Filtering material in its preparation method, its ceramic filtering device is made up of loose ceramic microsphere particle, single ceramic microballoon
Particle has interconnected air hole structure, its spherical grain structure has good structural stability, it is to avoid existing many
The shortcoming that hole ceramic material mechanical strength is not high, is difficult to, easily cracks.Ceramic filter can heatproof to 1000 DEG C of left sides
The right side, and decay resistance is good, but need periodic blowback to vibrate in its high-temperature gas separation process, ceramics itself
Thermal shock resistance and compression shock intensity are poor in addition for red brittleness, it is impossible to ensure the reliability of porous filter material in use.
High-temperature dust removal technological development research must try to achieve the efficient of chemical industry and other a variety of industrial circles with high start
Benefit, low energy consumption and the discharge of the low no three wastes, reach energy-conservation, environmental protection, and greatly simplification of flowsheet, reduce dust to equipment
Ground weares and teares, so that the purpose in extension device life-span.The present invention reacts synthetically prepared Ni-Cr- using element powders vacuum-sintering
Al-Y porous alloys, internal void is abundant uniform, and open porosity is high, improves filter efficiency；It is high temperature resistant, anti-oxidant, corrosion-resistant
Deng premium properties, it is ensured that the stability of filtering；Thermal shock resistance is good, high mechanical strength, solderable, easy to process.This hair
The service life of bright extension filter element effective while improving filtering accuracy and ensureing filtering stability.
The content of the invention
The invention discloses a kind of preparation method of new type high temperature dusty gas separation membrane-porous material, its specific preparation method
Comprise the following steps：
（1）Powder is prepared：Tetra- kinds of element powders of Ni, Cr, Al, Y are prepared by a certain percentage, wherein Cr, Al, Y powder are accounted for altogether always contains
The 20.5-47wt % of amount；
（2）Powder-processed：The powder prepared is placed on the mixed powder machine of V-type and at the uniform velocity mixed after 8-14h, powder gross mass 1- is added
3% stearic acid, then the dry 6-12h in 35-55 DEG C of common drying box；
（3）Pressure forming：By well mixed powder under 50-150MPa pressure after pressurize 10-90s it is compressing, obtain
Green compact；
（4）Green sintering：By step（3）Made green compact, which are placed in vacuum sintering furnace, to be sintered, and vacuum is 1 × 10-2-1×
10-3Pa；Sintering process is：Green compact are placed in vacuum drying oven, keep 5-10 DEG C/min programming rate to rise to 60-100 from room temperature
DEG C, it is incubated 90-120min；Then 300-400 DEG C is warming up to 3-6 DEG C/min programming rate, is incubated 90-120min；Then
550-650 DEG C is warming up to 1-5 DEG C/min programming rate, 180-240min is incubated；The last heating speed with 5-10 DEG C/min
Degree is warming up to 1100-1300 DEG C, is incubated 120-180min；Cool to room temperature with the furnace, that is, obtain invented high-temperature dusty gas
Separation membrane-porous material.
Preferably, step（1）Described in Ni powder powder diameter be 150-350 mesh, percentage is 53-79.5wt%, purity
For more than 99.5%.
Preferably, step（1）Described in Cr powder powder diameter be 150-350 mesh, percentage is 15-25wt%, and purity is
More than 99.5%.
Preferably, step（1）Described in Al powder powder diameter be 150-350 mesh, percentage is 5-20wt%, and purity is
More than 99.5%.
Preferably, step（1）Described in Y powder powder diameter be 200-300 mesh, percentage is 0.5-2wt%, and purity is
More than 99.5%.
The present invention is using the advantage of above-mentioned technical proposal：
（1）The present invention reacts synthetically prepared porous Ni-Cr-Al-Y alloys using element powders vacuum-sintering, and its pore-creating mechanism is
Violent diffusion pore-creating and high temperature sintering stage between powder particle mesopore in pressing process, the Ni/Al near Al fusing points
Ni and interphase spread pore-creating.The present invention can be realized high by controlling Particle Sizes, pressing pressure, sintering process
The hole of warm dusty gas separating and filtering element is controllable, orients and filters for the grit in varigrained flue gas, it is ensured that mistake
Filter precision.
（2）The porous material of the present invention selects the nickel itself with excellent anticorrosive performance as alloy substrate, with the addition of
The Cr and Al of high level, enable alloy surface to form good Al2O3And Cr2O3Oxide film, further prevents oxygen
To the oxidation of matrix, alloy is protected, prevent High Temperature Oxidation acceleration, base caused by the generation because of internal oxidition
Body penalty；The micro Y of addition, promotes Al2O3And Cr2O3The selective oxidation of film;Reduce Al2O3Or Cr2O3's
The speed of growth;Improve Al2O3Or Cr2O3The antistrip performance of film.On the basis of corrosion resistance is ensured, effectively increase
High temperature oxidation resistance, it is ensured that the stability of filtering.
（3）The present invention prepare porous Ni-Cr-Al-Y alloys, with excellent thermal shock resistance, higher mechanical strength,
It is solderable, it is not only easy to process, and effectively extend filter element service life.
（4）The present invention uses near-net-shape, and utilization rate of raw materials is high, preparing cost, low, technique is briefly controllable, and produces
During there is no the generation of industrial wastewater and waste gas, it is economic and environment-friendly, be adapted to industrial-scale production.
Brief description of the drawings
Fig. 1 is the surface topography map of the Ni-Cr-Al-Y porous materials prepared in embodiment 1.
Fig. 2 be in embodiment 1 the Ni-Cr-Al-Y porous materials that prepare at 800 DEG C oxidation weight gain with oxidization time t's
Change curve.
Fig. 3 be in embodiment 1 the Ni-Cr-Al-Y porous materials that prepare at 800 DEG C（Δm/m0）2With oxidization time t's
Graph of a relation.
Embodiment
With reference to specific embodiment, the invention will be further described.
Embodiment 1
Tetra- kinds of powder of Ni, Cr, Al, Y are prepared in proportion, wherein Ni contents are 79.5wt%, powder diameter is 350 mesh；Cr contents
For 15wt%, powder diameter is 350 mesh；Al content is 5wt%, and powder diameter is 350 mesh；Y contents are 0.5wt%, and powder diameter is
300 mesh.The powder prepared is placed on the stearic acid that powder gross mass 3% is added after 8h is at the uniform velocity mixed on the mixed powder machine of V-type, then
12h is dried in 35 DEG C of common drying boxes, with 50MPa pressure cold-press moulding, the dwell time is about 90s；Pressed compact is placed in vacuum
It is sintered in sintering furnace, vacuum is 5 × 10-3 Pa；Sintering process is：5 DEG C/min programming rate is kept to be risen to from room temperature
60 DEG C, it is incubated 120min；Then 300 DEG C are warming up to 3 DEG C/min programming rate, are incubated 120min；Then with 1 DEG C/min's
Programming rate is warming up to 550 DEG C, is incubated 240min；The last programming rate with 5 DEG C/min is warming up to 1100 DEG C, insulation
180min；Cool to room temperature with the furnace, that is, obtain invented high-temperature dusty gas separation membrane-porous material.
The micromorphology figure of resulting materials is as shown in figure 1, Ni-Cr-Al-Y porous materials have abundant linked hole
Gap, and even pore distribution；Its maximum diameter of hole is 10 μm, and open porosity is 42.5%, and gas permeability is 450m3m-2KP-1h-1。
In order to which researching high-temperature dusty gas separates the high in actual working environment moderate resistance of porous Ni-Cr-Al-Y alloy materials
Warm oxidation susceptibility.The sample for firing formation is placed in acetone soln and is cleaned through ultrasonic washing instrument device and is placed on corundum crucible
High-temperature heating removal of impurities for a long time is carried out in high temperature furnace, the sample after cleaning measures its original weight after fully drying, then by sample
Product, which are put in corundum crucible, is placed in the cyclic oxidation 480h at a temperature of 800 DEG C that is rapidly heated in stove.Every one in oxidizing process
The fixed time takes out sample and weighed, and takes three samples weigh averaging every time, to obtain the oxidation kinetics of material
Learn curve map 2 and Fig. 3.As shown in Fig. 2 initially increase is very fast for the quality of Ni-Cr-Al-Y porous materials, growth over time
In the trend being slowly increased.As shown in figure 3, by oxidation kinetics equation (Δ m/m0)2=KpT, (wherein Δ m is increased to aoxidize
Quality, m0For the original quality of sample, KpFor oxidation rate) calculate Ni-Cr-Al-Y at 800 DEG C oxidation rate be 9.97
×10-7%2/h。
Embodiment 2
Tetra- kinds of powder of Ni, Cr, Al, Y are prepared in proportion, wherein Ni contents are 53wt%, powder diameter is 150 mesh；Cr contents are
25wt%, powder diameter is 150 mesh；Al content is 20wt%, and powder diameter is 150 mesh；Y contents are 2wt%, and powder diameter is 200
Mesh.The powder prepared is placed on the stearic acid that powder gross mass 2% is added after 14h is at the uniform velocity mixed on the mixed powder machine of V-type, then 55
6h is dried in DEG C common drying box, with 150MPa pressure cold-press moulding, the dwell time is about 30s；Pressed compact is placed in into vacuum to burn
It is sintered in freezing of a furnace, vacuum is 1 × 10-2 Pa；Sintering process is：7 DEG C/min programming rate is kept to be risen to from room temperature
100 DEG C, it is incubated 100min；Then 400 DEG C are warming up to 4 DEG C/min programming rate, are incubated 100min；Then with 3 DEG C/min
Programming rate be warming up to 650 DEG C, be incubated 180min；The last programming rate with 7 DEG C/min is warming up to 1300 DEG C, insulation
120min；Cool to room temperature with the furnace, that is, obtain invented high-temperature dusty gas separation membrane-porous material.According in embodiment 1
Method carries out identical experiment, obtains the result similar to embodiment 1.
Embodiment 3
Tetra- kinds of powder of Ni, Cr, Al, Y are prepared in proportion, wherein Ni contents are 69wt%, powder diameter is 275 mesh；Cr contents are
20wt%, powder diameter is 275 mesh；Al content is 10wt%, and powder diameter is 275 mesh；Y contents are 1wt%, and powder diameter is 250
Mesh.The powder prepared is placed on the stearic acid that powder gross mass 1% is added after 10h is at the uniform velocity mixed on the mixed powder machine of V-type, then 50
8h is dried in DEG C common drying box, with 100MPa pressure cold-press moulding, the dwell time is about 50s；Pressed compact is placed in into vacuum to burn
It is sintered in freezing of a furnace, vacuum is 8 × 10-3 Pa；Sintering process is：10 DEG C/min programming rate is kept to be risen to from room temperature
80 DEG C, it is incubated 90min；Then 350 DEG C are warming up to 6 DEG C/min programming rate, are incubated 90min；Then with 5 DEG C/min liter
Warm speed is warming up to 600 DEG C, is incubated 200min；The last programming rate with 10 DEG C/min is warming up to 1200 DEG C, is incubated 140min；
Cool to room temperature with the furnace, that is, obtain invented high-temperature dusty gas separation membrane-porous material.Carried out according to the method in embodiment 1
Identical experiment, obtains the result similar to embodiment 1.
Embodiment 4
Tetra- kinds of powder of Ni, Cr, Al, Y are prepared in proportion, wherein Ni contents are 65.5wt%, powder diameter is 200 mesh；Cr contents
For 18wt%, powder diameter is 200 mesh；Al content is 15wt%, and powder diameter is 200 mesh；Y contents are 1.5wt%, powder diameter
For 200 mesh.The powder prepared is placed on the stearic acid that powder gross mass 2.5% is added after 12h is at the uniform velocity mixed on the mixed powder machine of V-type,
10h is dried in 40 DEG C of common drying boxes again, with 150MPa pressure cold-press moulding, the dwell time is about 10s；Pressed compact is placed in
It is sintered in vacuum sintering furnace, vacuum is 1 × 10-3 Pa；Sintering process is：8 DEG C/min programming rate is kept from room temperature
90 DEG C are risen to, 90min is incubated；Then 370 DEG C are warming up to 5 DEG C/min programming rate, are incubated 110min；Then with 2 DEG C/
Min programming rate is warming up to 620 DEG C, is incubated 220min；The last programming rate with 8 DEG C/min is warming up to 1250 DEG C, insulation
150min；Cool to room temperature with the furnace, that is, obtain invented high-temperature dusty gas separation membrane-porous material.According in embodiment 1
Method carries out identical experiment, obtains the result similar to embodiment 1.
Described above is only the better embodiment to the present invention, not makees any formal limit to the present invention
System, any simple modification that every technical spirit according to the present invention is made to embodiment of above, equivalent variations and modification,
Belong in the range of technical solution of the present invention.
Claims (3)
1. a kind of high-temperature dusty gas separates the preparation method of porous Ni-base alloy material, it is characterised in that comprise the following steps：
（1）Powder is prepared：Element powders of the tetra- kinds of purity of Ni, Cr, Al, Y more than 99.5% are prepared by a certain percentage, wherein
Cr, Al, Y powder account for the 20.5-47wt % of total content altogether；
（2）Powder-processed：The powder prepared is placed on the mixed powder machine of V-type and at the uniform velocity mixed after 8-14h, powder gross mass 1- is added
3% stearic acid, then the dry 6-12h in 35-55 DEG C of common drying box；
（3）Pressure forming：By well mixed powder under 50-150MPa pressure after pressurize 10-90s it is compressing, obtain
Green compact；
（4）Green sintering：By step（3）Made green compact, which are placed in vacuum sintering furnace, to be sintered, and vacuum is 1 × 10-2-1×
10-3Pa；Sintering process is：Green compact are placed in vacuum drying oven, keep 5-10 DEG C/min programming rate to rise to 60-100 from room temperature
DEG C, it is incubated 90-120min；Then 300-400 DEG C is warming up to 3-6 DEG C/min programming rate, is incubated 90-120min；Then
550-650 DEG C is warming up to 1-5 DEG C/min programming rate, 180-240min is incubated；The last heating speed with 5-10 DEG C/min
Degree is warming up to 1100-1300 DEG C, is incubated 120-180min；Cool to room temperature with the furnace, that is, obtain invented high-temperature dusty gas
Separation membrane-porous material.
2. as the preparation method of the new type high temperature dusty gas separation membrane-porous material described in claim 1, it is characterised in that step
（1）Described in element powders configuration proportion be：Ni, 53-79.5wt%；Cr, 15-25wt%；Al, 5-20wt%；Y, 0.5-2wt%.
3. as the preparation method of the new type high temperature dusty gas separation membrane-porous material described in claim 1, it is characterised in that step
（1）Described in element powders granularity it is as follows：Ni, 150-350 mesh；Cr, 150-350 mesh；Al, 150-350 mesh；Y, 200-300
Mesh.
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| CN108163903A (en) * | 2018-03-19 | 2018-06-15 | 浙江大学 | The spherical method for intersecting nickel hydroxide nano piece is prepared based on porous one step of nickel skeleton |
| CN108380882A (en) * | 2018-02-05 | 2018-08-10 | 湘潭大学 | A kind of Ni-Cr-Al-Cu porous materials and preparation method thereof |
| CN109454231A (en) * | 2018-12-18 | 2019-03-12 | 湖北汽车工业学院 | A kind of preparation method of iron aluminium copper micropore filter material |
| CN110125392A (en) * | 2019-06-28 | 2019-08-16 | 安泰环境工程技术有限公司 | A kind of outer light Fe-Al intermetallic compound filter element of high throughput and preparation method thereof |
| CN111450783A (en) * | 2020-04-08 | 2020-07-28 | 广州赛隆增材制造有限责任公司 | Preparation method of modified evaporation wall for supercritical water oxidation reactor |
| CN112403105A (en) * | 2020-10-30 | 2021-02-26 | 西北有色金属研究院 | Low-roughness small-aperture stainless steel porous sheet and preparation method thereof |
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| CN108380882B (en) * | 2018-02-05 | 2020-12-18 | 湘潭大学 | Ni-Cr-Al-Cu porous material and preparation method thereof |
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| CN109454231A (en) * | 2018-12-18 | 2019-03-12 | 湖北汽车工业学院 | A kind of preparation method of iron aluminium copper micropore filter material |
| CN109454231B (en) * | 2018-12-18 | 2021-02-05 | 湖北汽车工业学院 | Preparation method of iron-aluminum-copper alloy microporous filter material |
| CN110125392A (en) * | 2019-06-28 | 2019-08-16 | 安泰环境工程技术有限公司 | A kind of outer light Fe-Al intermetallic compound filter element of high throughput and preparation method thereof |
| CN110125392B (en) * | 2019-06-28 | 2022-02-15 | 安泰环境工程技术有限公司 | High-flux external light Fe-Al intermetallic compound filter element and preparation method thereof |
| CN111450783A (en) * | 2020-04-08 | 2020-07-28 | 广州赛隆增材制造有限责任公司 | Preparation method of modified evaporation wall for supercritical water oxidation reactor |
| CN111450783B (en) * | 2020-04-08 | 2022-02-01 | 广州赛隆增材制造有限责任公司 | Preparation method of modified evaporation wall for supercritical water oxidation reactor |
| CN112403105A (en) * | 2020-10-30 | 2021-02-26 | 西北有色金属研究院 | Low-roughness small-aperture stainless steel porous sheet and preparation method thereof |
| CN112403105B (en) * | 2020-10-30 | 2022-04-29 | 西北有色金属研究院 | Low-roughness small-aperture stainless steel porous sheet and preparation method thereof |
| CN115491563A (en) * | 2022-09-19 | 2022-12-20 | 中南大学 | Novel MAX phase porous material resistant to strong acid corrosion and preparation method thereof |
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