CN107299254B - 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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- 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 a kind of preparation methods of high-temperature dusty gas separation porous Ni-base alloy material.Preparation method of the invention is mainly that the compounding of (1) powder: 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, is dry, through cold moudling green compact；(3) green compact are carried out to the sintering of four stages in vacuum sintering furnace.The present invention reacts the Ni-Cr-Al-Y porous alloy being synthetically prepared using element powders vacuum-sintering, and internal void is abundant uniformly, and open porosity is high, filter efficiency is high, and there is excellent high temperature resistant, anti-oxidant, anti-thermal shock and corrosion resistance, high mechanical strength can weld, easy to process.The present invention effectively extends the service life of filter element while improving filtering accuracy and guaranteeing filtering stability.
Description
Technical field
The present invention relates to a kind of preparation methods of porous material, and in particular to is reacted and is synthesized by element powders vacuum-sintering
A kind of preparation method of high-temperature dusty gas separation porous Ni-base alloy material, belongs to air contaminant treatment dedusting technology field.
Background technique
Hot gas filtration technology can improve energy farthest using the physical sensible heat of gas, potential chemical heat
Source utilization rate, process simplification save equipment investment；Meanwhile it also avoiding carrying out flue gas cooling treatment and again wet process is removed
Secondarily polluted water brought by dirt.Therefore, rationally there is very huge economic value and social benefit using the technology.High temperature
Filter generally realizes the circular regeneration of filter element 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.Since the temperature of purge gas will be lower than filtering when reverse gas cleaning
The temperature of gas, filter bears rapid heating and cooling and the stress that generates, therefore requires 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 chimney filter is required to have good filterability.
(3) good high temperature resistant and corrosion resistance.Filter is generally in high temperature (800-1100 DEG C), high pressure (1.0-3.0MPa), strong
Acid, containing long-term work under the environment such as steam, oxygen-containing, working condition is very severe, therefore requires excellent high temperature resistant and resistance to
Corrosive nature.Sack cleaner becomes most widely used filter collector due to its high-effective dust-removing the characteristics of.Such as patent of invention
CN105080222A discloses a kind of pre- dedusting cooling device of bag filter, which is equipped with drop in pre-duster box house
Warm water tube greatly reduces the temperature of flue gas, reduces large dust particle or stone enters bag filter, to a certain extent
Extend the service life of cloth bag.However, since the cloth bags such as terylene, fiber material is easy hair in the dusty gas of strong corrosive
It phenomena such as heat contracting, degradation, oxidation, causes the reduction of filtering accuracy and reduces 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 higher filtering
Efficiency, and on the market filter exist mostly high temperature oxidation resistance is poor, corrosion resistance is insufficient, switching performance is poor,
The problems such as thermal shock resistance difference or low mechanical strength, develop a kind of high filtering precision and high-temperature filter with long service life have very much must
It wants.
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 more
Two class rigid filtration material of mesoporous metal and micropore ceramics.Patent of invention CN102895809A disclose a kind of ceramic filtering device and
Preparation method, the filtering material in ceramic filtering device is made of loose ceramic microsphere particle, single ceramic microballoon
Particle has interconnected air hole structure, and spherical grain structure has good structural stability, avoids existing more
Hole ceramic material mechanical strength is not high, is difficult to, is easy to produce the shortcomings that crackle.Ceramic filter can heatproof to 1000 DEG C of left sides
The right side, and corrosion resistance is good, but needs periodic blowback to vibrate in its high-temperature gas separation process, ceramics itself
Heat resistanceheat resistant vibration property and compression shock intensity are poor in addition for red brittleness, not can guarantee the reliability of porous filter material in use.
High-temperature dust removal technological development research must acquire the efficient of chemical industry and other a variety of industrial circles with high start
Beneficial, low energy consumption and the three wastes low/no discharge reaches energy conservation, environmental protection, and greatly simplification of flowsheet, reduces dust to equipment
Ground abrasion, to extend the purpose of equipment life.The present invention reacts the Ni-Cr- being synthetically prepared using element powders vacuum-sintering
Al-Y porous alloy, internal void is abundant uniformly, and open porosity is high, improves filter efficiency；It is high temperature resistant, anti-oxidant, corrosion-resistant
Equal excellent performances, ensure that the stability of filtering；Thermal shock resistance is good, high mechanical strength, can weld, easy to process.This hair
The bright service life for effectively extending filter element while improving filtering accuracy and guaranteeing filtering stability.
Summary of the invention
The invention discloses a kind of preparation method of high-temperature dusty gas separation membrane-porous material, specific preparation method includes
Following steps:
(1) powder is prepared: tetra- kinds of element powders of Ni, Cr, Al, Y being prepared by a certain percentage, wherein Cr, Al, Y powder account for altogether
The 20.5-47wt% of total content；
(2) powder-processed: prepared powder is placed on after at the uniform velocity mixing 8-14h on the mixed powder machine of V-type, the total matter of powder is added
The stearic acid of 1-3% is measured, then the dry 6-12h in 35-55 DEG C of normal drying case；
(3) pressure forming: the powder compression moulding after pressure maintaining 10-90s under the pressure of 50-150MPa that will be uniformly mixed,
Obtain green compact；
(4) green sintering: step (3) made green compact being placed in vacuum sintering furnace and are sintered, and vacuum degree is 1 × 10-2-
1×10-3Pa；Sintering process are as follows: green compact are placed in vacuum drying oven, the heating rate of 5-10 DEG C/min is kept to rise to 60- from room temperature
100 DEG C, keep the temperature 90-120min；Then it is warming up to 300-400 DEG C with the heating rate of 3-6 DEG C/min, keeps the temperature 90-120min；So
It is warming up to 550-650 DEG C with the heating rate of 1-5 DEG C/min afterwards, keeps the temperature 180-240min；Finally with the heating of 5-10 DEG C/min
Speed is warming up to 1100-1300 DEG C, keeps the temperature 120-180min；Room temperature is cooled to the furnace to get to the high temperature dust gas invented
Body separation membrane-porous material.
Preferably, the powder diameter of Ni powder described in step (1) is 150-350 mesh, and percentage 53-79.5wt% is pure
Degree is 99.5% or more.
Preferably, the powder diameter of Cr powder described in step (1) is 150-350 mesh, percentage 15-25wt%, purity
It is 99.5% or more.
Preferably, the powder diameter of Al powder described in step (1) is 150-350 mesh, and percentage 5-20wt%, purity is
99.5% or more.
Preferably, the powder diameter of Y powder described in step (1) is 200-300 mesh, and percentage 0.5-2wt%, purity is
99.5% or more.
The present invention by adopting the above technical scheme the advantages of be:
(1) present invention is synthetically prepared porous Ni-Cr-Al-Y alloy, borer using element powders vacuum-sintering reaction
Reason is the violent diffusion pore-creating and high temperature sintering between powder particle mesopore in pressing process, the Ni/Al near Al fusing point
The Ni and interphase in stage spread pore-creating.The present invention can be real by controlling Particle Sizes, pressing pressure, sintering process
The hole of existing high-temperature dusty gas separating and filtering element is controllable, orients filtering for the grit in varigrained flue gas, protects
Demonstrate,prove filtering accuracy.
(2) porous material of the invention selects the nickel with excellent anticorrosive performance itself as alloy substrate, is added to
The Cr and Al of high level, make alloy surface be capable of forming good Al2O3And Cr2O3Oxide film further prevents oxygen pair
The oxidation of matrix, protects alloy, prevents High Temperature Oxidation acceleration, matrix caused by the generation because of internal oxidition
Penalty；Micro Y is added, Al is promoted2O3And Cr2O3The selective oxidation of film；Reduce Al2O3Or Cr2O3Growth speed
Degree；Improve Al2O3Or Cr2O3The antistrip performance of film.On the basis of guaranteeing corrosion resistance, oxygen resistant to high temperatures is effectively increased
Change performance, ensure that the stability of filtering.
(3) present invention prepare porous Ni-Cr-Al-Y alloy, with excellent thermal shock resistance, higher mechanical strength,
It is solderable, it is not only easy to process, but also effectively extend filter element service life.
(4) present invention uses near-net-shape, and utilization rate of raw materials is high, preparation cost is low, technique is briefly controllable, and produces
It is economic and environment-friendly in the process without the generation of industrial wastewater and exhaust gas, it is suitble to industrial-scale production.
Detailed description of the invention
Fig. 1 is the surface topography map of the Ni-Cr-Al-Y porous material prepared in embodiment 1.
Fig. 2 be in embodiment 1 the Ni-Cr-Al-Y porous material for preparing at 800 DEG C oxidation weight gain with oxidization time t's
Change curve.
Fig. 3 is the Ni-Cr-Al-Y porous material for preparing (the Δ m/m at 800 DEG C in embodiment 10)2With oxidization time t's
Relational graph.
Specific embodiment
The invention will be further described combined with specific embodiments below.
Embodiment 1
Tetra- kinds of powder of Ni, Cr, Al, Y are prepared in proportion, wherein Ni content is 79.5wt%, and powder diameter is 350 mesh；
Cr content is 15wt%, and powder diameter is 350 mesh；Al content is 5wt%, and powder diameter is 350 mesh；Y content is 0.5wt%,
Powder diameter is 300 mesh.Prepared powder is placed on after at the uniform velocity mixing 8h on the mixed powder machine of V-type and total powder quality 3% is added
Stearic acid, then the dry 12h in 35 DEG C of normal drying casees, with the pressure cold-press moulding of 50MPa, the dwell time is about 90s；It will pressure
Base is placed in vacuum sintering furnace and is sintered, and vacuum degree is 5 × 10-3Pa；Sintering process are as follows: keep the heating rate of 5 DEG C/min
60 DEG C are risen to from room temperature, keeps the temperature 120min；Then 300 DEG C are warming up to the heating rate of 3 DEG C/min, keep the temperature 120min；Then
550 DEG C are warming up to the heating rate of 1 DEG C/min, keeps the temperature 240min；Finally 1100 are warming up to the heating rate of 5 DEG C/min
DEG C, keep the temperature 180min；Room temperature is cooled to the furnace to get to the high-temperature dusty gas separation membrane-porous material invented.
The micromorphology figure of resulting materials is as shown in Figure 1, Ni-Cr-Al-Y porous material has linked hole abundant
Gap, and even pore distribution；Its maximum diameter of hole is 10 μm, open porosity 42.5%, gas permeability 450m3m-2KP-1h-1。
In order to which researching high-temperature dusty gas separates the anti-height in actual working environment of porous Ni-Cr-Al-Y alloy material
Warm oxidation susceptibility.The sample for firing formation is placed in acetone soln and is cleaned through ultrasonic cleaning instrument and is placed on corundum crucible
High temperature furnace is interior to carry out high-temperature heating removal of impurities for a long time, and the sample after cleaning measures its original weight after sufficiently 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 furnace.Every one in oxidation process
The fixed time takes out sample and weighs, and takes three samples to carry out weighing every time and is averaged, to obtain the oxidation kinetics of material
Learn curve graph 2 and Fig. 3.As shown in Fig. 2, the quality of Ni-Cr-Al-Y porous material initially increases comparatively fast, with the growth of 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 that oxidation is increased
Quality, m0For the original quality of sample, KpFor oxidation rate) be calculated 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 content is 53wt%, and powder diameter is 150 mesh；Cr
Content is 25wt%, and powder diameter is 150 mesh；Al content is 20wt%, and powder diameter is 150 mesh；Y content is 2wt%, powder
Partial size is 200 mesh.Prepared powder is placed on to the tristearin that total powder quality 2% is added after at the uniform velocity mixing 14h on the mixed powder machine of V-type
Acid, then the dry 6h in 55 DEG C of normal drying casees, with the pressure cold-press moulding of 150MPa, the dwell time is about 30s；Green compact is set
It is sintered in vacuum sintering furnace, vacuum degree is 1 × 10-2Pa；Sintering process are as follows: keep the heating rate of 7 DEG C/min from room
Temperature rise keeps the temperature 100min to 100 DEG C；Then 400 DEG C are warming up to the heating rate of 4 DEG C/min, keep the temperature 100min；Then with 3
DEG C/heating rate of min is warming up to 650 DEG C, keep the temperature 180min；1300 DEG C finally are warming up to the heating rate of 7 DEG C/min, is protected
Warm 120min；Room temperature is cooled to the furnace to get to the high-temperature dusty gas separation membrane-porous material invented.According in embodiment 1
Method carry out identical experiment, obtain and result similar in embodiment 1.
Embodiment 3
Tetra- kinds of powder of Ni, Cr, Al, Y are prepared in proportion, wherein Ni content is 69wt%, and powder diameter is 275 mesh；Cr
Content is 20wt%, and powder diameter is 275 mesh；Al content is 10wt%, and powder diameter is 275 mesh；Y content is 1wt%, powder
Partial size is 250 mesh.Prepared powder is placed on to the tristearin that total powder quality 1% is added after at the uniform velocity mixing 10h on the mixed powder machine of V-type
Acid, then the dry 8h in 50 DEG C of normal drying casees, with the pressure cold-press moulding of 100MPa, the dwell time is about 50s；Green compact is set
It is sintered in vacuum sintering furnace, vacuum degree is 8 × 10-3Pa；Sintering process are as follows: keep the heating rate of 10 DEG C/min from room
Temperature rise keeps the temperature 90min to 80 DEG C；Then 350 DEG C are warming up to the heating rate of 6 DEG C/min, keep the temperature 90min；Then with 5 DEG C/
The heating rate of min is warming up to 600 DEG C, keeps the temperature 200min；1200 DEG C finally are warming up to the heating rate of 10 DEG C/min, heat preservation
140min；Room temperature is cooled to the furnace to get to the high-temperature dusty gas separation membrane-porous material invented.According in embodiment 1
Method carries out identical experiment, obtains and result similar in embodiment 1.
Embodiment 4
Tetra- kinds of powder of Ni, Cr, Al, Y are prepared in proportion, wherein Ni content is 65.5wt%, and powder diameter is 200 mesh；
Cr content is 18wt%, and powder diameter is 200 mesh；Al content is 15wt%, and powder diameter is 200 mesh；Y content is 1.5wt%,
Powder diameter is 200 mesh.Prepared powder is placed on after at the uniform velocity mixing 12h on the mixed powder machine of V-type and total powder quality 2.5% is added
Stearic acid, then the dry 10h in 40 DEG C of normal drying casees, with the pressure cold-press moulding of 150MPa, the dwell time is about 10s；
Green compact is placed in vacuum sintering furnace and is sintered, vacuum degree is 1 × 10-3Pa；Sintering process are as follows: keep the heating of 8 DEG C/min
Speed rises to 90 DEG C from room temperature, keeps the temperature 90min；Then 370 DEG C are warming up to the heating rate of 5 DEG C/min, keep the temperature 110min；So
620 DEG C are warming up to the heating rate of 2 DEG C/min afterwards, keeps the temperature 220min；Finally 1250 are warming up to the heating rate of 8 DEG C/min
DEG C, keep the temperature 150min；Room temperature is cooled to the furnace to get to the high-temperature dusty gas separation membrane-porous material invented.According to implementation
Method in example 1 carries out identical experiment, obtains and result similar in embodiment 1.
The above is only not to make limit in any form to the present invention to better embodiment of the invention
System, any simple modification that embodiment of above is made according to the technical essence of the invention, equivalent variations and modification,
Belong in the range of technical solution of the present invention.
Claims (2)
1. a kind of preparation method of high-temperature dusty gas separation porous Ni-base alloy material, it is characterised in that the following steps are included:
(1) powder is prepared: tetra- kinds of purity of Ni, Cr, Al, Y are prepared by a certain percentage in 99.5% or more element powders, wherein
Ni, 53-79.5wt%；Cr, 15-25wt%；Al, 5-20wt%；Y, 0.5-2wt%；
(2) powder-processed: prepared powder is placed on after at the uniform velocity mixing 8-14h on the mixed powder machine of V-type, total powder quality 1- is added
3% stearic acid, then the dry 6-12h in 35-55 DEG C of normal drying case；
(3) pressure forming: uniformly mixed powder compression moulding after pressure maintaining 10-90s under the pressure of 50-150MPa obtains
Green compact；
(4) green sintering: step (3) made green compact being placed in vacuum sintering furnace and are sintered, and vacuum degree is 1 × 10-2-1×
10-3Pa；Sintering process are as follows: green compact are placed in vacuum drying oven, the heating rate of 5-10 DEG C/min is kept to rise to 60-100 from room temperature
DEG C, keep the temperature 90-120min；Then it is warming up to 300-400 DEG C with the heating rate of 3-6 DEG C/min, keeps the temperature 90-120min；Then
It is warming up to 550-650 DEG C with the heating rate of 1-5 DEG C/min, keeps the temperature 180-240min；Finally with the heating speed of 5-10 DEG C/min
Degree is warming up to 1100-1300 DEG C, keeps the temperature 120-180min；It is porous to get separating to high-temperature dusty gas to cool to room temperature with the furnace
Material.
2. by the preparation method of high-temperature dusty gas separation membrane-porous material described in claim 1, which is characterized 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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| CN108380882B (en) * | 2018-02-05 | 2020-12-18 | 湘潭大学 | Ni-Cr-Al-Cu porous material and preparation method thereof |
| CN108163903B (en) * | 2018-03-19 | 2019-10-22 | 浙江大学 | The spherical method for intersecting nickel hydroxide nano piece is prepared based on porous one step of nickel skeleton |
| 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 |
| 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 |
| 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 |
| 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 |
| CN115491563B (en) * | 2022-09-19 | 2023-05-26 | 中南大学 | MAX phase porous material resistant to strong acid corrosion and preparation method thereof |
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| TWI259849B (en) * | 2001-06-11 | 2006-08-11 | Sumitomo Electric Industries | Porous metal, metallic composite using it and method for manufacturing the same |
| US20080175885A1 (en) * | 2007-01-19 | 2008-07-24 | Cinvention Ag | Porous, degradable implant made by powder molding |
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| US3964877A (en) * | 1975-08-22 | 1976-06-22 | General Electric Company | Porous high temperature seal abradable member |
| CN102492865A (en) * | 2011-12-01 | 2012-06-13 | 西北有色金属研究院 | Porous material for purifying high-temperature gas and preparation method thereof |
| CN105780048A (en) * | 2016-04-08 | 2016-07-20 | 湘潭大学 | Preparation method for novel porous electrolysis hydrogen evolution cathode material |
| CN106191505A (en) * | 2016-07-08 | 2016-12-07 | 湘潭大学 | A kind of preparation method of new type high temperature antioxidation porous material |
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