CN100336588C - Process for regenerating sulfur loading active carbon - Google Patents
Process for regenerating sulfur loading active carbon Download PDFInfo
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- CN100336588C CN100336588C CNB2004100796489A CN200410079648A CN100336588C CN 100336588 C CN100336588 C CN 100336588C CN B2004100796489 A CNB2004100796489 A CN B2004100796489A CN 200410079648 A CN200410079648 A CN 200410079648A CN 100336588 C CN100336588 C CN 100336588C
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- Prior art keywords
- active carbon
- carrier gas
- regeneration
- gas
- sulfur loading
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 31
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 16
- 239000011593 sulfur Substances 0.000 title claims abstract description 16
- 238000011068 loading method Methods 0.000 title claims description 13
- 230000001172 regenerating effect Effects 0.000 title abstract description 10
- 239000012159 carrier gas Substances 0.000 claims abstract description 38
- 230000008929 regeneration Effects 0.000 claims abstract description 36
- 238000011069 regeneration method Methods 0.000 claims abstract description 36
- 239000007789 gas Substances 0.000 claims abstract description 22
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims description 9
- 238000003795 desorption Methods 0.000 claims description 9
- 238000009418 renovation Methods 0.000 claims description 9
- 229940099596 manganese sulfate Drugs 0.000 claims description 5
- 235000007079 manganese sulphate Nutrition 0.000 claims description 5
- 239000011702 manganese sulphate Substances 0.000 claims description 5
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 5
- 239000002594 sorbent Substances 0.000 claims description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- 239000006199 nebulizer Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 239000008246 gaseous mixture Substances 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- 229940072033 potash Drugs 0.000 claims description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 2
- 235000015320 potassium carbonate Nutrition 0.000 claims description 2
- 229960001781 ferrous sulfate Drugs 0.000 claims 1
- 230000009719 regenerative response Effects 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 9
- 238000011084 recovery Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 9
- 238000001179 sorption measurement Methods 0.000 description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 4
- 239000002156 adsorbate Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 210000000952 spleen Anatomy 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010327 methods by industry Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Separation Of Gases By Adsorption (AREA)
Abstract
The present invention relates to a method for regenerating active carbon with sulfur, particularly to a method for regenerating by desorbing active carbon with sulfur in a microwave heating mode. The present invention comprises: dry and pure carbon dioxide carrier gas enters a reactor positioned in the center of the top of a microwave oven under the controlled pressure; the desorbing regeneration is carried out under the conditions that the ratio of microwave power to the amount of the active carbon is 4 to 20 W/g, the pressure of the carrier gas is 10 to 100 mmH2O, the flow rate of the carrier gas is 0.45 to 0.8 m/s, the regeneration time of the microwaves is 2 to 5 min, and the rated frequency of the microwave oven is 915MHz to 2450MHz; sulfur is desorbed in the form of SO2 so that the active carbon is regenerated, and the carrier gas with the SO2 content of 30 to 90% at the outlet can be used as raw gas for preparing sulfuric acid.
Description
(1) technical field: active carbon regeneration.
(2) background technology
Active carbon is because its unique physical arrangement and excellent adsorption performance are widely used in fields such as water treatment, chemical industry and environmental protection.For a long time, people have carried out a large amount of research to the renovation process of active carbon, proposed various process engineering for regenerating, main renovation process has at present: chemical removal method, bioanalysis, wet oxidation process, electrochemical process, heating etc., and wherein with the heating best results.The new renovation process that grew up in recent years has: high-frequency impulse method, above-critical state carbon dioxide process, supercritical ultrasonics technology etc.The known regeneration techniques that is applied to desulphurized aetivated carbon mainly contains three kinds: high temperature inert gas regeneration, high-temperature vapor pyrolysis regeneration, washing regeneration.But the utilization with regard to the maturity of technology, product waits, and high temperature regeneration is undoubtedly because of its product utilization is alternative greatly, non-secondary pollution is more promising, but traditional heating regeneration is heat medium with hot-air and steam usually.But this method recovery time is long, the general 1h～6h that gets, and the shortest 0.5h that also wants, the heat energy utilization rate is low, and the active carbon loss is high, and regeneration back Properties of Activated Carbon recovery rate is low, owing to operation at high temperature, the high material consumption of regenerating furnace; Operating condition (humidity, time, and the quantity of oxidizing gas) must strict control, and cost of equipment is big etc.
The applicant is disclosed a kind of with microwave heating method regeneration year volatile nonpolar organic matter process of active carbon in patent No. ZL00113039.0 title " method of regeneration, by micro-wave, of active carbon loading voltile and nonpolar organic matter ", because heating using microwave speed is fast, homogeneous heating, thermograde is little, heat simultaneously the inside and outside when being used for active carbon regeneration, heat transfer direction and characteristics such as the mass transfer direction is consistent, the applicant is applied in the regenerated carbon, and the applicant it is essential in regenerative process and improves desorption rate and reduce the proportion of goods damageds of active carbon and regeneration rate and the adsorption capacity that improves active carbon in this patent of invention.The factor that influences them mainly contains microwave power, amounts of activated carbon, recovery time and flow rate of carrier gas etc., the technical scheme that proposes in this patent is: control its flow and pressure from the carrier gas that the carrier gas source of the gas comes out after preliminary treatment, enter the active carbon regeneration reactor that is positioned at microwave applicator, to the active carbon processing of regenerating, work off one's feeling vent one's spleen and handle reuse through cooling, its process conditions are microwave power and the ratio of amounts of activated carbon is 70～90W/g, flow rate of carrier gas is 0.1～0.3m/s, recovery time 6～7min, carrier gas is an inert gas.
Disclosed in the patent application of German patent DE 3834831 is a kind of carbon filter regeneration technology and equipment, and the purpose of its invention is that its technology path is the composition structure of research regenerating unit by the method regeneration filtrate with the heating using microwave filtering material; Disclosed gaseous organic substance adsorption method in the text of U.S. Pat 6022399A, its objective is that seeking a kind of adsorbent comes nonpolar organic matter in the Purge gas, research is to the modification of adsorbent, result of study has proposed the employing hydrophobic zeolite as adsorbent, and absorbs in addition modification of solids with microwave.
The present invention is on the basis of the ZL00113039.0 patented technology of the applicant's application, launches the achievement that research obtains at the characteristics of sulfur loading active carbon regeneration.
(3) summary of the invention
The objective of the invention is to adopt the method for heating using microwave, to carrying the regeneration of sulfur absorbent active carbon, adopt carbon dioxide as carrier gas, and control its flow and pressure enters the active carbon regeneration reactor that is positioned at microwave applicator, sulfur loading active carbon is regenerated, work off one's feeling vent one's spleen and after the cooling cooling, can be used as the unstripped gas of preparation sulfuric acid.
Fig. 1 is flow path device figure of the present invention.
The important indicator that active carbon regeneration needs to consider is a desorption rate, the adsorption capacity of regenerated carbon and the active carbon proportion of goods damageds, influence factor to these indexs is an amounts of activated carbon, the microwave desorption efficiency, microwave irradiation time, and select suitable carrier gas etc., at the characteristics of sulfur loading active carbon desorb, propose the process conditions of following parsing regeneration sulfur loading active carbon among the present invention: microwave power is 4～20W/g with the ratio of amounts of activated carbon, and nebulizer gas pressure is: 20～100mmH
2O, flow rate of carrier gas is: 0.45～0.8m/s, the micro wave regeneration time is: 2～5min, carrier gas is a carbon dioxide.Result of study shows: (1) microwave power is big more, and desorption effect is good more, SO in the stripping gas
2Concentration high more; (2) by the impregnation technology appendix can improve SO in the stripping gas after the activated carbon of sorbent desorb of metal ion
2Concentration, with the manganese sulfate [Mn (SO of mass percent 1.2%
4)
2] dipping the active carbon desorption effect best; (3) increase of flow rate of carrier gas can reduce the recovery time, but has reduced outlet SO simultaneously
2Concentration, this technology determine that 0.5m/s is best flow rate of carrier gas.
The present invention finishes according to the following steps:
1) the dry and purification of carrier gas carbon dioxide gas
The pressure of control carrier gas is 20～100mmH
2O, flow rate of carrier gas 0.45～0.8m/s, at first with silica dehydrator, purification carrier gas, be dried to the carrier gas water content and be lower than 5%, and remove the impurity such as dust in the carrier gas, guarantee to make the carrier gas of dried and clean under the pressure of control, to enter the reactor that is arranged in the micro-wave oven center of top.
2) microwave desorption and regeneration part: carrier gas 8 enters the reactor 3 that is arranged in the micro-wave oven center of top after flowmeter 7 meterings, carry out the reaction of sulfur loading active carbon desorption and regeneration, micro-wave oven rated frequency 915MHz～2450MHz, microwave power is 4-20W/g with the ratio of amounts of activated carbon, and nebulizer gas pressure is 20～100mmH
2O, flow rate of carrier gas are 0.45～0.8m/s, recovery time 2-5min, and top arm 9 and cooling tower join, and are loaded with SO from what reactor came out
2Carrier gas is connected to cooling tower 2, and thermocouple inserts reactor from the aperture of crown center.Adsorb saturated active carbon, following reaction take place during desorb:
SO
2 *→SO
2 (1)
SO
2 *+C→S+CO
2 (2)
SO
2 *+2C→S+2CO (3)
SO
2Be polar molecule, energy strong absorption microwave, SO
2 *SO behind the finger absorption microwave
2Molecule.
3) SO
2Recovery: contain SO from being loaded with of coming out of reactor
2Temperature Deng gaseous mixture reaches 150 ℃, must be cooled to 30～40 ℃ by cooling tower earlier, the high concentration SO of outlet 30～90%
2Send through vavuum pump 1, can be used as the unstripped gas of preparation sulfuric acid.
Activated carbon of sorbent can adopt potash (K earlier
2CO
3), ferrous sulfate (FeSO
4), cobalt acetate [Co (AC)
2], copper nitrate [Cu (NO
3)
2] or manganese sulfate [Mn (SO
4)
2] one of in four kinds of solution to its flood, drying makes.This adsorbent is used for SO
2Adsorption cleaning, the adsorbent that adsorbs after saturated is regenerated with the method for microwave irradiation.Appendix can make SO in the stripping gas during active carbon microwave irradiation desorb of above metal ion
2Concentration improve 20～50%.
Compare the present invention to have firing rate fast with known technology, regenerated carbon adsorption capacity height, SO
2The desorption rate height, the active carbon proportion of goods damageds are low, SO in the stripping gas
2The high advantage of concentration.
(4) description of drawings: Fig. 1 is flow path device figure of the present invention.1 is vavuum pump among the figure, the 2nd, and cooler, the 3rd, micro-wave oven, the 4th, reactor, the 5th, thermocouple, the 6th, magnetoelectricity, the 7th, flowmeter, the 8th, carrier gas, the 9th, top arm, T are valves, P is a Pressure gauge.
(5) specific embodiment:
Embodiment one:
Adopt above-mentioned technological process, carrier gas is a carbon dioxide gas, adopt flowmeter meter flow, Pressure gauge is measured pressure, microwave applicator is rated output power 1400W (adjustable power) micro-wave oven, and regeneration reactor is made (high 520mm, diameter 120mm) by quartz glass, the active carbon of handling of regenerating is the charcoal granular active carbon, with the manganese sulfate [Mn (SO of mass percent 1.2%
4)
2] it is flooded, adsorbate is SO
2, active carbon is to SO
2Adsorption capacity be 0.41kgSO
2/ kg active carbon.
Technological condition of regeneration is: flow rate of carrier gas 0.5m/s, amounts of activated carbon 138.2g, microwave power 1400W, recovery time 5min.
Active carbon regeneration rate 95%, SO in the stripping gas
2Concentration 75%.
Embodiment two
Adopt above-mentioned technological process, carrier gas is a carbon dioxide gas, adopt flowmeter meter flow, Pressure gauge instrumentation level pressure power, microwave applicator is rated output power 1400W (adjustable power) micro-wave oven, and regeneration reactor is made (high 260mm, diameter 50mm) by quartz glass, the active carbon of handling of regenerating is a powdered activated carbon, with the copper nitrate [Cu (NO of mass percent 0.5%
3)
2] it is flooded, adsorbate is SO
2, active carbon is to SO
2Adsorption capacity be 0.38kgSO
2/ kg active carbon.
Technological condition of regeneration is: flow rate of carrier gas 0.8m/s, amounts of activated carbon 50g, microwave power 700W, recovery time 4min.
Active carbon regeneration rate 88%, SO in the stripping gas
2Concentration 70%.
Embodiment three
Adopt above-mentioned technological process, carrier gas is a carbon dioxide gas, adopt flowmeter meter flow, Pressure gauge is measured pressure, microwave applicator is rated output power 200W (adjustable power) micro-wave oven, and regeneration reactor is made (high 260mm, diameter 50mm) by quartz glass, the activity of handling of regenerating is the charcoal granular active carbon, and adsorbate is SO
2, active carbon is to SO
2Adsorption capacity be 0.34kgSO
2/ kg active carbon.
Technological condition of regeneration is: flow rate of carrier gas 0.45m/s, amounts of activated carbon 50g, microwave power 200W, recovery time 5min.
Active carbon regeneration rate 86%, SO in the stripping gas
2Concentration 70%.
Claims (5)
1, a kind of renovation process of sulfur loading active carbon, the carrier gas of dried and clean enters the reactor that is arranged in the micro-wave oven center of top under the pressure of control, carry out the active carbon desorption regenerative response, the carrier gas of coming out from reactor after the desorb, by cooling tower cooling, it is characterized in that carrier gas is a carbon dioxide gas, technological condition of regeneration is a microwave power and the ratio of amounts of activated carbon is 4～20W/g, and nebulizer gas pressure is 20～100mmH
2O, flow rate of carrier gas are 0.45～0.8m/s, and the micro wave regeneration time is 2～5min, micro-wave oven rated frequency 915MHz～2450MHz.
2, the renovation process of sulfur loading active carbon according to claim 1 is characterized in that, carrier gas is dried to water content and is lower than 5%.
3, the renovation process of sulfur loading active carbon according to claim 1 and 2 is characterized in that, goes out to suck SO
2The temperature of gaseous mixture reaches 150 ℃, must be cooled to 30～40 ℃ by cooling tower earlier, and carrier gas contains the SO of 30～90% concentration
2Send through vavuum pump (1), as the unstripped gas of preparation sulfuric acid.
4, the renovation process according to claim 1 or 2 or 3 described sulfur loading active carbons is characterized in that, activated carbon of sorbent adopt in potash, ferrous sulfate, cobalt acetate, copper nitrate, the manganese sulfate a kind of solution to its flood, drying makes.
5, the renovation process of sulfur loading active carbon according to claim 4 is characterized in that, with the manganese sulfate dipping activated carbon of sorbent of mass percent 1.2%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100796489A CN100336588C (en) | 2004-12-30 | 2004-12-30 | Process for regenerating sulfur loading active carbon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100796489A CN100336588C (en) | 2004-12-30 | 2004-12-30 | Process for regenerating sulfur loading active carbon |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1669639A CN1669639A (en) | 2005-09-21 |
| CN100336588C true CN100336588C (en) | 2007-09-12 |
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ID=35041204
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|---|---|---|---|
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100372605C (en) * | 2006-01-16 | 2008-03-05 | 史鱼海 | Movable sulfurization active carbon heating regenerator and regeneration |
| CN103007677A (en) * | 2012-12-24 | 2013-04-03 | 上海克硫环保科技股份有限公司 | Movable desorption and regeneration system and method for active coke |
| CN103230786B (en) * | 2013-05-07 | 2015-12-16 | 南京工业大学 | Activated carbon regeneration adsorption device and process thereof |
| CN104388111B (en) * | 2014-11-30 | 2016-04-06 | 东北电力大学 | A kind of recovery process of microwave adsorption desorption oil shale distillation gas lightweight oil |
| CN104479726B (en) * | 2014-11-30 | 2016-05-18 | 东北电力大学 | A kind of retracting device of microwave adsorption desorption oil shale retorting gas light oil |
| CN110841725A (en) * | 2019-11-04 | 2020-02-28 | 上海环钻环保科技股份有限公司 | Microwave regeneration treatment method of carbon-based catalyst for simultaneous desulfurization and denitrification |
| CN113877553B (en) * | 2021-10-27 | 2024-01-23 | 中冶赛迪技术研究中心有限公司 | Active carbon regeneration process for desulfurization of blast furnace gas |
| CN113856657A (en) * | 2021-11-08 | 2021-12-31 | 田世超 | Method for recovering manganese and ammonium salt from activated carbon for producing manganese product and method for regenerating activated carbon |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6022399A (en) * | 1997-06-27 | 2000-02-08 | Daimler Chrysler Ag. | Process for the adsorption of organic substances in the air |
| CN1136965C (en) * | 2000-06-16 | 2004-02-04 | 昆明理工大学 | Method for regeneration, by micro-wave, of active carbon loading voltile and nonpolar organic matter |
-
2004
- 2004-12-30 CN CNB2004100796489A patent/CN100336588C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6022399A (en) * | 1997-06-27 | 2000-02-08 | Daimler Chrysler Ag. | Process for the adsorption of organic substances in the air |
| CN1136965C (en) * | 2000-06-16 | 2004-02-04 | 昆明理工大学 | Method for regeneration, by micro-wave, of active carbon loading voltile and nonpolar organic matter |
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|---|---|
| CN1669639A (en) | 2005-09-21 |
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