CN103937558B - Based on desulfurizing agent for high-temp gas preparation method in microwave radiation - Google Patents
Based on desulfurizing agent for high-temp gas preparation method in microwave radiation Download PDFInfo
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- CN103937558B CN103937558B CN201410154584.8A CN201410154584A CN103937558B CN 103937558 B CN103937558 B CN 103937558B CN 201410154584 A CN201410154584 A CN 201410154584A CN 103937558 B CN103937558 B CN 103937558B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 230000003009 desulfurizing effect Effects 0.000 title claims abstract description 16
- 230000005855 radiation Effects 0.000 title claims abstract description 7
- 239000003765 sweetening agent Substances 0.000 claims abstract description 34
- 235000003599 food sweetener Nutrition 0.000 claims abstract description 33
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 claims abstract description 12
- 229940007718 zinc hydroxide Drugs 0.000 claims abstract description 12
- 229910021511 zinc hydroxide Inorganic materials 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 238000004898 kneading Methods 0.000 claims description 2
- 238000003801 milling Methods 0.000 claims description 2
- 238000003746 solid phase reaction Methods 0.000 claims description 2
- 238000010671 solid-state reaction Methods 0.000 claims description 2
- 238000006477 desulfuration reaction Methods 0.000 abstract description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052717 sulfur Inorganic materials 0.000 abstract description 8
- 239000011593 sulfur Substances 0.000 abstract description 8
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000011800 void material Substances 0.000 abstract description 2
- 239000003463 adsorbent Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 17
- 238000002156 mixing Methods 0.000 description 12
- 230000023556 desulfurization Effects 0.000 description 10
- 239000000126 substance Substances 0.000 description 9
- 238000000498 ball milling Methods 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 239000003245 coal Substances 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000007493 shaping process Methods 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 239000003034 coal gas Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002309 gasification Methods 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 238000005987 sulfurization reaction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- BPJYAXCTOHRFDQ-UHFFFAOYSA-L tetracopper;2,4,6-trioxido-1,3,5,2,4,6-trioxatriarsinane;diacetate Chemical class [Cu+2].[Cu+2].[Cu+2].[Cu+2].CC([O-])=O.CC([O-])=O.[O-][As]1O[As]([O-])O[As]([O-])O1.[O-][As]1O[As]([O-])O[As]([O-])O1 BPJYAXCTOHRFDQ-UHFFFAOYSA-L 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000012958 reprocessing Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of based on desulfurizing agent for high-temp gas preparation method in microwave radiation, is adopt zinc hydroxide and Red Stone Ware to be raw material, fires standby middle desulfurizing agent for high-temp gas through a step microwave heating baking.The present invention adopts has plasticity-is good, void content is high, cohesiveness is strong Red Stone Ware as sweetening agent carrier, and the desulfurizing adsorbent of preparation is good, and physical strength is excellent, its physical strength 150 ~ 250N/cm, single Sulfur capacity more than 18%, desulfuration efficiency more than 98%.
Description
Technical field
The present invention relates to gas desulfurizer preparing technical field, be specifically related to the preparation method of desulfurizing agent for high-temp gas in a kind of Zinc oxide-base.
Background technology
Gasification of coal, as important coal cleaning conversion technology, plays an important role in the field such as production chemical industry synthetic gas (synthetic ammonia, methyl alcohol), industrial fuel gas, town gas.Gasification of coal can not only significantly improve utilising efficiency and the thermo-efficiency of Coal Clean conversion, and environmental friendliness.Sulphur in feed coal about 80% changes into H in gasification of coal gas-making process
2s enters coal gas, H
2the existence of S not only can cause the corrosion of equipment, pipeline and internal combustion turbine, and can make poisoning of catalyst, and serious harm HUMAN HEALTH, therefore to remove it.
H in the industrial application coal gas such as general internal combustion turbine
2s content requirement is less than 20ppm, has the H of the synthesis gas of sulfur resistant catalyst
2s content at 100 ~ 200ppm, and is used as the H of synthesis unstripped gas
2s content then must lower than 0.1ppm.Reach the oligosaprobic production standard of these low emissions, the preparation of efficient desulfurizing agent and selection are crucial steps.
Coal gas desulfurization technology is mainly divided into wet desulphurization and dry desulfurization two kinds.Wet Flue Gas Desulfurization Technique is ripe, and treatment capacity is large, can operate continuously, and running cost is lower, is widely used, and be used for the thick de-of hydrogen sulfide, but gas heat loss is comparatively large in sweetening process, thermo-efficiency is low, there is the problems such as sewage disposal.Comparatively speaking, dry desulfurization process simplification, easy to operate, equipment is simple, and load is little, saves sensible heat, increases generating output rating, all has comparatively high purification to organosulfur and inorganic sulfur, is suitable for the meticulous desulfurization of process lean sulphurous gas, particularly gas.
Zinc oxide is just widely used in field of Environment Protection at the beginning of last century, in waste water control and air contaminant treatment, achieved good effect.Especially, in desulfurization, zinc oxide, as sweetening agent, is widely used in (as fields such as chemical industry, petrochemical complex, oil refining, beverages) especially.Zinc oxide-base gas desulfurizer has the advantages such as desulfurization precision is high, Sulfur capacity is large, easy to use, stable and reliable for performance, is the focus that people study always.
CN 102703134A discloses a kind of method utilizing desulfurizing agent for high-temp gas in microwave radiation preparation.This invention utilizes microwave heating baking to fire standby sweetening agent, and its single Sulfur capacity is more than 25%, and use through ten sulfurations/reprocessing cycle, Sulfur capacity still remains on more than 20%, and still keeps higher physical strength after circulation ten times.CN 102489107A discloses the method for a kind of microwave intermitant irradiation active carbon desulfurization denitration.This invention utilizes microwave exposure activated carbon granule, be adsorbed on the sulphur oxynitride of activated carbon surface, at high temperature be decomposed into elemental sulfur and nitrogen by charcoal fast restore, greatly can reduce the energy consumption of microwave exposure, reduce charcoal loss, realize the in-situ regeneration of gac, have that removal effect is good, the regeneration of activated carbon time is short, remove that cost is low, the rate of recovery is high, be easy to the features such as industrializing implementation.
China's Red Stone Ware huge number, widely distributed, its mineral products mainly concentrate on the south of the lower reaches of the Yangtze River.The mineral type of each producing region Red Stone Ware is different with chemical constitution, shows different physics and chemistry character.Jiangsu's Red Stone Ware is well-known at home and abroad with the uniqueness of himself, SiO in yixing purple sand soil
2content 55 ~ 65%, Al
2o
3content 22 ~ 31%, SiO
2/ Al
2o
3ratio 1.82 ~ 2.90, Fe
2o
3content relatively high (about 8%), other oxide compounds (Na
2o, MgO, K
2o, CaO, TiO
2) content less and among a small circle change, there is the features such as green strength is high, shrinkability is little, plasticity-is strong, void content is high, iron-holder is high, cohesiveness is good.
Summary of the invention
The object of this invention is to provide a kind of based on desulfurizing agent for high-temp gas preparation method in microwave radiation, the sweetening agent physical strength prepared in the process of the present invention is excellent.
The middle desulfurizing agent for high-temp gas preparation method that the present invention is based on microwave radiation be with zinc hydroxide and Red Stone Ware for raw material, utilize solid-state reaction under microwave to prepare sweetening agent.
Red Stone Ware mixes with the mass ratio of zinc hydroxide according to 1 ︰ 1 ~ 2.5 by concrete preparation method of the present invention, is ground to 60 ~ 100 orders.Abrasive adds water kneading, and after extrusion, drying forming, microwave calcining 15 ~ 60min at 500 ~ 600 DEG C, makes desulfurizing agent for high-temp gas in Zinc oxide-base.
Wherein, described Red Stone Ware is preferably Jiangsu's Red Stone Ware, its SiO
2content 56 ~ 63wt%, Al
2o
3content 22 ~ 30wt%, SiO
2/ Al
2o
3ratio 1.87 ~ 2.86, Fe
2o
3content 3.0% ~ 9.0wt%.
In aforesaid method of the present invention, use micro-wave frequency for 2450MHz.
In aforesaid method, described grinding is preferably carried out in ball milling instrument, milling time 1 ~ 4h, ball milling instrument rotating speed preferably 200 ~ 500r/min.
In aforesaid method, described oven dry dries 1 ~ 2h at 80 ~ 100 DEG C in an oven.
Red Stone Ware containing 30 ~ 55wt% in desulfurizing agent for high-temp gas in Zinc oxide-base prepared by aforesaid method of the present invention, is mainly used in middle high temperature coal gas purification field, desulfurization temperature 450 ~ 600 DEG C.
Preparation method of the present invention is with zinc hydroxide and Red Stone Ware for raw material, and a step microwave heating baking fires standby middle desulfurizing agent for high-temp gas, and process is simple, substantially reduces preparation time, and operation is convenient controlled, and environmental pollution is little, overcomes the agglomeration traits that solution method is brought.Particularly the present invention adopts Red Stone Ware as the carrier of sweetening agent, can be good at the pore volume and the physical strength that strengthen sweetening agent, the sweetening agent of preparation has the features such as selectivity is good, Active components distribution is even, physical strength is excellent, sweetening agent physical strength 150 ~ 250N/cm, single Sulfur capacity more than 18%, desulfuration efficiency more than 98%.
Embodiment
Embodiment 1
Select Ding Shu town, Yixing this mountain green mud of Huanglong Mountain Red Stone Ware as sweetening agent carrier, its SiO
2content 61.41%, Al
2o
3content 24.01%, SiO
2/ Al
2o
3ratio 2.56, Fe
2o
3content 3.45%.
Take zinc hydroxide 50 grams, Red Stone Ware 50 grams, put into ball milling instrument after mixing, grind 2 hours with the rotating speed of 400r/min, add deionized water mixing, extruded moulding.Baking oven put into by sample after shaping, dries 1 hour, makes the bar shaped sweetening agent of diameter 3mm, long 3mm for 80 DEG C.Proceed in crucible, at frequency 2450MHz, under the microwave condition of power 500W, be warming up to 500 DEG C of roastings 1 hour, make sweetening agent finished product A, main physico-chemical property is in table 1.
Embodiment 2
Select Ding Shu town, Yixing this mountain green mud of Huanglong Mountain Red Stone Ware as sweetening agent carrier, its SiO
2content 61.41%, Al
2o
3content 24.01%, SiO
2/ Al
2o
3ratio 2.56, Fe
2o
3content 3.45%.
Take zinc hydroxide 60 grams, Red Stone Ware 50 grams, put into ball milling instrument after mixing, grind 3 hours with the rotating speed of 400r/min, add deionized water mixing, extruded moulding; Baking oven put into by sample after shaping, dries 1 hour, makes the bar shaped sweetening agent of diameter 3mm, long 3mm for 80 DEG C.Proceed in crucible, at frequency 2450MHz, under the microwave condition of power 600W, be warming up to 500 DEG C of roasting 45min, make sweetening agent finished product B, main physico-chemical property is in table 1.
Embodiment 3
Select Huanglong Mountain Red Stone Ware purple mud in Ding Shu town, Yixing as sweetening agent carrier, its SiO
2content 60.30%, Al
2o
3content 25.66%, SiO
2/ Al
2o
3ratio 2.35, Fe
2o
3content 8.70%.
Take zinc hydroxide 75 grams, Red Stone Ware 50 grams, put into ball milling instrument after mixing, grind 2 hours with the rotating speed of 350r/min, add deionized water mixing, extruded moulding; Baking oven put into by sample after shaping, dries 1 hour, makes the bar shaped sweetening agent of diameter 3mm, long 3mm for 80 DEG C.Proceed in crucible, at frequency 2450MHz, under the microwave condition of power 700W, be warming up to 550 DEG C of roasting 45min, make sweetening agent finished product C, main physico-chemical property is in table 1.
Embodiment 4
Select Huanglong Mountain Red Stone Ware purple mud in Ding Shu town, Yixing as sweetening agent carrier, its SiO
2content 60.30%, Al
2o
3content 25.66%, SiO
2/ Al
2o
3ratio 2.35, Fe
2o
3content 8.70%.
Take zinc hydroxide 100 grams, Red Stone Ware 50 grams, put into ball milling instrument after mixing, grind 3 hours with the rotating speed of 350r/min, add deionized water mixing, extruded moulding; Baking oven put into by sample after shaping, dries 1 hour, makes the bar shaped sweetening agent of diameter 3mm, long 3mm for 80 DEG C.Proceed in crucible, at frequency 2450MHz, under the microwave condition of power 800W, be warming up to 550 DEG C of roasting 30min, make sweetening agent finished product D, main physico-chemical property is in table 1.
Embodiment 5
Select Ding Shu town, Yixing Huanglong Mountain Red Stone Ware red soil as sweetening agent carrier, its SiO
2content 62.15%, Al
2o
3content 22.34%, SiO
2/ Al
2o
3ratio 2.78, Fe
2o
3content 6.93%.
Take zinc hydroxide 110 grams, Red Stone Ware 50 grams, put into ball milling instrument after mixing, grind 2 hours with the rotating speed of 300r/min, add deionized water mixing, extruded moulding; Baking oven put into by sample after shaping, dries 1 hour, makes the bar shaped sweetening agent of diameter 3mm, long 3mm for 80 DEG C.Proceed in crucible, at frequency 2450MHz, under the microwave condition of power 900W, be warming up to 600 DEG C of roasting 30min, make sweetening agent finished product E, main physico-chemical property is in table 1.
Embodiment 6
Select Ding Shu town, Yixing Huanglong Mountain Red Stone Ware red soil as sweetening agent carrier, its SiO
2content 62.15%, Al
2o
3content 22.34%, SiO
2/ Al
2o
3ratio 2.78, Fe
2o
3content 6.93%.
Take zinc hydroxide 125 grams, Red Stone Ware 50 grams, put into ball milling instrument after mixing, grind 3 hours with the rotating speed of 300r/min, add deionized water mixing, extruded moulding; Baking oven put into by sample after shaping, dries 1 hour, makes the bar shaped sweetening agent of diameter 3mm, long 3mm for 80 DEG C.Proceed in crucible, at frequency 2450MHz, under the microwave condition of power 900W, be warming up to 600 DEG C of roasting 15min, make sweetening agent finished product F, main physico-chemical property is in table 1.
*---sweetening agent Sulfur capacity appreciation condition: desulfurization temperature 550 DEG C, air speed 2000
-1, entrance H
2s concentration 2500ppm.X
1, X
2, X
3(X=A, B, C, D, E, F) represents a sulfuration respectively, post cure and three sulfurations.
Claims (6)
1. based on desulfurizing agent for high-temp gas preparation method in microwave radiation, for raw material with zinc hydroxide and Red Stone Ware, solid-state reaction under microwave is utilized to prepare sweetening agent, Red Stone Ware is it is characterized in that to mix with the mass ratio of zinc hydroxide according to 1 ︰ 1 ~ 2.5, be ground to 60 ~ 100 orders, add water abrasive kneading, after extrusion, drying forming, microwave calcining 15 ~ 60min at 500 ~ 600 DEG C, makes desulfurizing agent for high-temp gas in Zinc oxide-base.
2. sweetening agent preparation method according to claim 1, is characterized in that described Red Stone Ware is Jiangsu's Red Stone Ware.
3. sweetening agent preparation method according to claim 1 and 2, is characterized in that SiO in described Red Stone Ware
2content 56 ~ 63wt%, Al
2o
3content 22 ~ 30wt%, SiO
2/ Al
2o
3ratio 1.87 ~ 2.86, Fe
2o
3content 3.0% ~ 9.0wt%.
4. sweetening agent preparation method according to claim 1 and 2, is characterized in that described microwave frequency 2450MHz.
5. sweetening agent preparation method according to claim 1, is characterized in that described milling time 1 ~ 4h.
6. desulfurizing agent for high-temp gas in preparing with claim 1,2 or 3 method, the Red Stone Ware containing 30 ~ 55wt% in described sweetening agent.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410154584.8A CN103937558B (en) | 2014-04-17 | 2014-04-17 | Based on desulfurizing agent for high-temp gas preparation method in microwave radiation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410154584.8A CN103937558B (en) | 2014-04-17 | 2014-04-17 | Based on desulfurizing agent for high-temp gas preparation method in microwave radiation |
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| Publication Number | Publication Date |
|---|---|
| CN103937558A CN103937558A (en) | 2014-07-23 |
| CN103937558B true CN103937558B (en) | 2015-09-30 |
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| CN106867593B (en) * | 2017-03-15 | 2019-12-06 | 太原理工大学 | Preparation method of Zn-Al hydrotalcite-based medium-high temperature gas desulfurizer |
| CN109999626A (en) * | 2019-04-30 | 2019-07-12 | 太原理工大学 | A method of preparing copper oxide/carbon nano-fiber flexible compound gas desulfurizer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1712500A (en) * | 2004-06-21 | 2005-12-28 | 煤炭科学研究总院 | High-temperature gas composite oxide desulfurizer and production thereof |
| CN102703134A (en) * | 2012-05-14 | 2012-10-03 | 太原理工大学 | Method for preparing medium-high temperature gas desulfurizing agent by microwave radiation |
-
2014
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1712500A (en) * | 2004-06-21 | 2005-12-28 | 煤炭科学研究总院 | High-temperature gas composite oxide desulfurizer and production thereof |
| CN102703134A (en) * | 2012-05-14 | 2012-10-03 | 太原理工大学 | Method for preparing medium-high temperature gas desulfurizing agent by microwave radiation |
Non-Patent Citations (2)
| Title |
|---|
| Regeneration characteristics and kinetics of Fe2O3/lignite semicoke hot gas desulfurizer at O2/N2 atmosphere;Xiurong Ren et al.;《J Therm Anal Calorim》;20140122;第116卷;1083-1090 * |
| Tunable Shape Microwave Synthesis of Zinc Oxide Nanospheres and Their Desulfurization Performance Compared with Nanorods and Platelet-Like Morphologies for the Removal of Hydrogen Sulfide;Hector F. G. et al.;《THE JOURNAL OF PHYSICAL CHEMISTRY C》;20120328;第116卷;8465-8474 * |
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