CN101703928A - Low-temperature carbonyl sulfide hydrolysis activated carbon-supported catalyst and preparation method thereof - Google Patents
Low-temperature carbonyl sulfide hydrolysis activated carbon-supported catalyst and preparation method thereof Download PDFInfo
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- CN101703928A CN101703928A CN200910095077A CN200910095077A CN101703928A CN 101703928 A CN101703928 A CN 101703928A CN 200910095077 A CN200910095077 A CN 200910095077A CN 200910095077 A CN200910095077 A CN 200910095077A CN 101703928 A CN101703928 A CN 101703928A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 32
- 230000007062 hydrolysis Effects 0.000 title claims abstract description 22
- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 title abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 56
- 238000000034 method Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012153 distilled water Substances 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 5
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 230000004913 activation Effects 0.000 claims description 4
- 239000002250 absorbent Substances 0.000 claims description 3
- 230000002745 absorbent Effects 0.000 claims description 3
- 239000003610 charcoal Substances 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 239000003245 coal Substances 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000005470 impregnation Methods 0.000 claims description 2
- 238000002803 maceration Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 9
- 238000006477 desulfuration reaction Methods 0.000 abstract description 4
- 230000023556 desulfurization Effects 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000003213 activating effect Effects 0.000 abstract 2
- 239000003513 alkali Substances 0.000 abstract 1
- 238000009835 boiling Methods 0.000 abstract 1
- 238000007654 immersion Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- 238000005303 weighing Methods 0.000 description 7
- 230000008859 change Effects 0.000 description 5
- 230000003009 desulfurizing effect Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 125000001741 organic sulfur group Chemical group 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- -1 EAC modified activated carbon Chemical class 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- GWZOLWLJEJRQMZ-UHFFFAOYSA-N [S].S Chemical compound [S].S GWZOLWLJEJRQMZ-UHFFFAOYSA-N 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000006552 photochemical reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- JOKPITBUODAHEN-UHFFFAOYSA-N sulfanylideneplatinum Chemical compound [Pt]=S JOKPITBUODAHEN-UHFFFAOYSA-N 0.000 description 1
- 230000019635 sulfation Effects 0.000 description 1
- 238000005670 sulfation reaction Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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Abstract
The invention relates to a preparation method of a low-temperature carbonyl sulfide hydrolysis activated carbon-supported catalyst. The method comprises the following steps: (1) grinding activated carbon, sieving the ground activated carbon to 40-60 meshes, washing for 3-4 times, then boiling for 1.5 h with l mol/L KOH solution, washing with distilled water until the pH value is constant, and then drying at the temperature of 120 DEG C for later use; (2) ultrasonic immersing the activated carbon in the step (1) with metal oxide immersion liquid with mass content accounting for 1-9 percent of that of the activated carbon for 30 min; (3) keeping the temperature of the activated carbon after immersing treatment in the step (2) constant for 3-6 h at the temperature of 120-170 DEG C, and then activating for 3 h at the temperature of 200-700 DEG C; and (4) ultrasonic immersing the activated carbon after activating in the step (3) with alkali solution with mass content accounting for 3-15 percent of that of the activated carbon for 30 min, and then keeping the temperature of the activated carbon constant for 3 h at the temperature of 110 DEG C to 160 DEG C to obtain the activated carbon-supported catalyst. The preparation method can remove the COS in the gas, simultaneously remove the H2S generated during the hydrolysis, has higher desulfurization precision, can obtain the low-cost raw material easily and also has the advantages of good activity at the normal and low temperature, low cost and the like.
Description
Technical field
The present invention relates to catalyst technical field, specifically a kind of low temperature hydrolysis cos (COS) carbon base catalyst and preparation method thereof and application.
Background technology
COS is the principal mode that organic sulfur exists in the industrial gasses, and the COS of trace is easy to cause the catalyst poisoning inactivation in the industrial production, and the equipment of industrial product is had corrosiveness.In addition, the not treated COS that is discharged in the atmosphere can form SO
2, promote photochemical reaction, and finally be converted into sulfate aerosol, bring serious environmental problem.Because chemism compares H
2S is much smaller, and its acidity and polarity all are weaker than H
2S generally is used to remove H
2The method of S can not remove COS effectively fully, is the key that realizes the smart desulfurization of gas so remove COS, has only to have solved removing of COS and just might make the total sulfur of industrial gasses reduce to instructions for use.In the sour gas processing procedure, removing of COS is more special, and conventional sulfur method is difficult to remove.The present technology that mainly removes has reducing process, Hydrolyze method, absorption process, absorption method, photodissociation method and oxidizing process etc.What research was many recently is Hydrolyze method, and its subtractive process is: COS+H
2O → CO
2+ H
2S under the effect of hydrolyst, utilizes the steam in tail gas or the unstripped gas that COS is changed into more tractable inorganic sulfur hydrogen sulfide, hydrogen sulfide is removed by other approach again.
At present both at home and abroad the patent of relevant carbonyl sulfide hydrolysis is a lot, is broadly divided into three classes according to its serviceability temperature: normal low temperature (room temperature～150 ℃) carbonyl sulfide hydrolysis catalysis patented technology, middle low temperature (80～250 ℃) carbonyl sulfide hydrolysis catalysis patented technology and middle temperature (200～400 ℃) carbonyl sulfide hydrolysis catalysis patented technology.
U.S. Pat P 4,455,446 disclose a kind of at γ-Al
2O
3The COS hydrolyst of last load platinum sulfide, weak point are catalyst cost height, and need regular regeneration.
U.S. Pat P4,5111,668 disclose a kind of with TiO
2Be carrier, contain a kind of alkali metal, alkaline-earth metal, IIB family and IVA family metal COS hydrolyst at least as active component.But the in use handled unstripped gas COS of this catalyst content lower (73ppm), and reaction temperature higher (200-400 ℃).
Japan Patent P0316,615, JP02,276,891 and the COS hydrolyst serviceability temperature that makes of Chinese patent CN921045247 greater than 40 ℃, only can transform COS is H
2S can not remove the H of generation
2S.CN93107483, the constant temperature fine desulfurizing technology that the COS hydrolyst string active carbon that 5 patents at first propose is formed, the fine desulfurizing technology index of the hydrolysis string normal temp zinc oxide that proposes than Britain ICI company is better, and investment can reduce by 1/2, uses in China tens pure factories of connection of family.
That the carrier of catalyst is selected for use basically in these patents is γ-Al
2O
3Or γ-Al
2O
3With TiO
2Complex carrier, and carrying alkali metal, alkaline-earth metal and transition metal oxide are made on these carriers.
In recent years, the Hubei Prov. Chemical Research Inst selected for use active carbon to make the COS hydrolyst as carrier.Patent CN96118013,7 disclose a kind of activated carbon desulphurization agent and preparation method, 0～100 ℃ of this catalyst serviceability temperature, air speed 100～3000h
-1, organic sulfur removal rate＞99%.Patent CN93107483,5 disclose a kind of constant temperature fine desulfurizing production technology.It is that process gas is passed through desulfurizing agent, again water or steam heater is heated to 40～80 ℃, is cooled to normal temperature by hydrolyst and cooling tower and realizes desulfurization.The desulfurizing agent that this process is selected for use is the EAC modified activated carbon, or iron oxide TG-1 type, SN-1 type etc.
Above-mentioned catalyst has following shortcoming: the temperature of (1) catalyzing hydrolysis is higher, and hydrolysis is an exothermic process, and equilibrium conversion is lower under the high temperature; (2) waste energy, investment is big, the operating cost height. and therefore, it is low to make Applicable temperature, removes the precision height, the equilibrium conversion height, it is very significant avoiding the sulfation fouled catalyst.
Summary of the invention
For overcoming the deficiency that existing catalyst exists, the invention provides a kind of low temperature hydrolysis cos (COS) carbon base catalyst and preparation method thereof and application, be mainly used in the cos that removes in the unstripped gas, it is good that this catalyst has a normal low temperature active, low cost and other advantages.
The objective of the invention is to realize by following method, this catalyst be with active carbon as carrier, the preparation method may further comprise the steps:
(1) active carbon is broken with the alms bowl grinding, and be sized to the 40-60 order, wash 3-4 time with running water and distillation respectively, the KOH solution with 1mol/L boils 1.5h then, and it is constant to be washed till pH with distilled water again, and the oven dry back is standby under 120 ℃ then;
(2) account for the active carbon 30min of 1～9% metal oxide impregnated liquid ultrasonic immersing (1) step of quality of activated carbon with mass content, maceration extract volume consumption is the maximum adsorption capacity of active carbon;
(3) active carbon that (2) step impregnation process is crossed constant temperature 3～6h under 120～170 ℃ of temperature conditions, and then under 200～700 ℃ of temperature, activate 3h;
(4) account for active carbon 30min after 3～15% aqueous slkali ultrasonic immersing (3) the step activation of quality of activated carbon with mass content, constant temperature 3h under 110～160 ℃ of temperature conditions promptly gets absorbent charcoal based catalyst then.
Described active carbon is commercially available coal mass active carbon (LJ-40).Used active carbon washing agent is running water and distilled water.Described metal oxide impregnated liquid is KMnO
4, Mn (CH
3COO)
2, MnSO
4In a kind of.Described dipping aqueous slkali is KOH, NaOH, Na
2CO
3, NaHCO
3, K
2CO
3, KHCO
3In a kind of.
The activity of such catalysts test is carried out in fixed bed reactors, and condition is reactor diameter 8mm, and the catalyst height is 4cm, and activity is represented with COS hydrolysis clearance.
The present invention uses 50 ℃, air speed 1000～3000h in minimum temperature
-1, during normal pressure, the COS in the gas can be removed the H that hydrolysis is produced simultaneously
2S removes in the lump, and desulfurization precision is higher, and unstripped gas need contain a certain amount of water, and raw material is cheap and easy to get, and it is good to have a normal low temperature active, low cost and other advantages.
Description of drawings
Describe the present invention in detail with drawings and Examples below.
Fig. 1, Fig. 2, Fig. 3, Fig. 4 and Fig. 5 are COS catalyzing hydrolysis efficient change curve in time.
The specific embodiment
(1), get 10g LJ-40 active carbon and grind brokenly with alms bowl, and be sized to the 40-60 order, with running water and distillation washing 3-4 time, the KOH solution with 1mol/L boils 1.5h then respectively, it is constant to be washed till pH with distilled water again, is placed on dry 3h in 120 ℃ of thermostatic drying chambers;
(2), take by weighing 0.16g KMnO
4Add in the 3ml distilled water, get pretreated active carbon 3g ultrasonic immersing 30min in (1) step;
(3), with Immesion active carbon 120 ℃ of dry 3h in thermostatic drying chamber of step (2), put into Muffle furnace then, at 300 ℃ of following activation 3h;
(4), take by weighing 0.29gKOH and add in the 3ml distilled water, the active carbon 30min after ultrasonic immersing step (3) activation, constant temperature 3h under 120 ℃ of temperature conditions promptly gets absorbent charcoal based catalyst then. the active testing reaction condition is: 50 ℃ of temperature, air speed 1000h
-1, COS concentration 1200mg/m
3, the reaction outlet does not detect H
2S, its activity is seen Fig. 1.
Embodiment 2
According to the method for embodiment 1, change takes by weighing KMnO
4Amount be 0.49g, take by weighing 0.55gKOH and obtain catalyst.The active testing reaction condition is: 50 ℃ of temperature, air speed 1000h
-1, COS concentration 1400mg/m
3, the reaction outlet does not detect H
2S, its activity is seen Fig. 2.
Embodiment 3
According to the method for embodiment 1, take by weighing 0.1g Na
2CO
3, the change sintering temperature is 700 ℃ and obtains catalyst.The active testing reaction condition is: 50 ℃ of temperature, air speed 1000h
-1, COS concentration 1400mg/m
3, the reaction outlet does not detect H
2S, its activity is seen Fig. 3.
Embodiment 4
Method according to embodiment 1 takes by weighing 0.24gNaHCO
3, the change baking temperature is 130 ℃ and obtains catalyst.Reaction condition is: 60 ℃ of temperature, air speed 1000h
-1, COS concentration 1600mg/m
3, the reaction outlet does not detect H
2S, its activity is seen Fig. 4.
Embodiment 5
According to the method for embodiment 1, change KMnO
4Be Mn (CH
3COO)
2And take by weighing 0.25g and prepare catalyst.Reaction condition is: 50 ℃ of temperature, air speed 1000h
-1, COS concentration 1300mg/m
3, the reaction outlet does not detect H
2S, its activity is seen Fig. 5.
Claims (6)
1. the preparation method of a low temperature hydrolysis cos carbon base catalyst is characterized in that carrying out according to the following steps:
(1) active carbon is broken with the alms bowl grinding, and be sized to the 40-60 order, wash 3-4 time with running water and distillation respectively, the KOH solution with 1mol/L boils 1.5h then, and it is constant to be washed till pH with distilled water again, and the oven dry back is standby under 120 ℃ then;
(2) account for the active carbon 30min of 1～9% metal oxide impregnated liquid ultrasonic immersing (1) step of quality of activated carbon with mass content, maceration extract volume consumption is the maximum adsorption capacity of active carbon;
(3) active carbon that (2) step impregnation process is crossed constant temperature 3～6h under 120～170 ℃ of temperature conditions, and then under 200～700 ℃ of temperature, activate 3h;
(4) account for active carbon 30min after aqueous slkali ultrasonic immersing (3) the step activation of 3-15% of quality of activated carbon with mass content, constant temperature 3h under 110～160 ℃ of temperature conditions promptly gets absorbent charcoal based catalyst then.
2. the preparation method of low temperature hydrolysis cos carbon base catalyst according to claim 1 is characterized in that described active carbon is commercially available coal mass active carbon LJ-40.
3. the preparation method of low temperature hydrolysis cos carbon base catalyst according to claim 1 is characterized in that described metal oxide impregnated liquid is KMnO
4, Mn (CH
3COO)
2, MnSO
4In a kind of.
4. the preparation method of low temperature hydrolysis cos carbon base catalyst according to claim 1 is characterized in that described dipping aqueous slkali is KOH, NaOH, Na
2CO
3, NaHCO
3, K
2CO
3, KHCO
3In a kind of.
5. press the low temperature hydrolysis cos carbon base catalyst that the described preparation method of claim 1 prepares for one kind.
6. press the application of the low temperature hydrolysis cos carbon base catalyst of the described preparation method's preparation of claim 1, it is characterized in that the active reaction condition is: COS concentration 1200-1400mg/m
3, 50 ℃ of temperature, air speed 1000h
-1
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350328A (en) * | 2011-07-26 | 2012-02-15 | 潘秋明 | Method for cleaning activated carbon |
| CN104931432A (en) * | 2015-06-30 | 2015-09-23 | 苏州东辰林达检测技术有限公司 | Carbon oxysulfide detection reagent and preparation method thereof |
| CN102600850B (en) * | 2012-01-13 | 2016-06-22 | 昆明理工大学 | A kind of preparation method of the catalyst of elimination cos and Carbon bisulfide simultaneously |
| CN106311245A (en) * | 2015-06-24 | 2017-01-11 | 云南民族大学 | Preparation method for lignite semi-coke-based denitration agent used for low-temperature catalytic oxidation |
| CN112206760A (en) * | 2019-07-11 | 2021-01-12 | 中国石化扬子石油化工有限公司 | High-activity carbonyl sulfide hydrolysis catalyst and preparation method thereof |
| CN113070032A (en) * | 2021-04-22 | 2021-07-06 | 浙江工业大学 | Amine functionalized activated carbon material and preparation method and application thereof |
| CN115106108B (en) * | 2021-03-18 | 2023-11-14 | 宝山钢铁股份有限公司 | COS hydrolysis catalyst for blast furnace gas and preparation method thereof |
-
2009
- 2009-10-22 CN CN200910095077A patent/CN101703928A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350328A (en) * | 2011-07-26 | 2012-02-15 | 潘秋明 | Method for cleaning activated carbon |
| CN102600850B (en) * | 2012-01-13 | 2016-06-22 | 昆明理工大学 | A kind of preparation method of the catalyst of elimination cos and Carbon bisulfide simultaneously |
| CN106311245A (en) * | 2015-06-24 | 2017-01-11 | 云南民族大学 | Preparation method for lignite semi-coke-based denitration agent used for low-temperature catalytic oxidation |
| CN104931432A (en) * | 2015-06-30 | 2015-09-23 | 苏州东辰林达检测技术有限公司 | Carbon oxysulfide detection reagent and preparation method thereof |
| CN112206760A (en) * | 2019-07-11 | 2021-01-12 | 中国石化扬子石油化工有限公司 | High-activity carbonyl sulfide hydrolysis catalyst and preparation method thereof |
| CN115106108B (en) * | 2021-03-18 | 2023-11-14 | 宝山钢铁股份有限公司 | COS hydrolysis catalyst for blast furnace gas and preparation method thereof |
| CN113070032A (en) * | 2021-04-22 | 2021-07-06 | 浙江工业大学 | Amine functionalized activated carbon material and preparation method and application thereof |
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