CN108246298A - A kind of method of nano lamellar solid base removing carbonyl sulfur - Google Patents
A kind of method of nano lamellar solid base removing carbonyl sulfur Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/308—Carbonoxysulfide COS
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Abstract
The present invention relates to a kind of method that nano lamellar solid base removes carbonyl sulfur in gas, the method for carbonyl sulfur is in this nano lamellar solid base removing gas：Carbonyl sulfur is 40 in temperature under the effect of nano lamellar catalyzed by solid base in industrial chemicals or tail gas of sulphuroC‑80oC, water and carbonyl sulfur molar ratio are 1.1:1‑2:1st, the material gas air speed containing COS is 1.0 4000h‑1Under conditions of, hydrolysis and oxidation reaction occurs, the oxidation through oxygen in water is converted into sulphur simple substance and sulfate after COS hydrolysis, realizes the removing of COS, and carbonyl sulfide removal rate is up to more than 99.5%；Nano lamellar solid base after inactivation regenerates after soda-dip, washing, drying and roasting, and the solid base after regeneration recycles.Nano lamellar oxide solid alkali prepared by the present invention, crystal size distribution range is relatively narrow, large specific surface area, and dispersion degree is high, and preparation process is simple.
Description
Technical field
The present invention relates to material gas or tail gas of sulphur removing organic sulfur fields, and in particular to a kind of nano lamellar solid
The method of carbonyl sulfur in alkali removing gas.
Background technology
With the rapid development of economy, energy supply and demand contradiction becomes increasingly conspicuous, it is scientific and reasonable to be received using the high sulfur-bearing energy
Extensive concern.The tail gas of sulphur in the material gas and follow-up desulfurization process prepared using coal, oil and natural gas as raw material
In containing a large amount of sulfide, be broadly divided into two major class of organic sulfur and inorganic sulfur, organic sulfur includes carbonyl sulfur, carbon disulfide, thiophene
Fen, mercaptan etc., inorganic sulfur is then primarily referred to as hydrogen sulfide.Wherein carbonyl sulfur accounts for the 80-90% of organic sulfur total amount, its presence is not only
The rotten candle of unstrpped gas pipeline is easily caused, reduces the service life of equipment, but also be easy to cause the poisoning of downstream catalyst,
Increase the cost of production therefore, the removing of carbonyl sulfur be during unstripped gas deep purifying the main problem to be solved in addition, making
For a kind of main organic sulfur in industrial gasses, the carbonyl sulfur in air is drained into anti-by a series of chemistry, photochemistry
Ying Houhui is generated, and is caused environmental pollution, is threatened the health and wellbeing of the mankind.Therefore, the removing research of carbonyl sulfur has important
Environment protection significance.
Currently used COS removal methods include reduction method, Hydrolyze method, absorption process, absorption method and oxidizing process etc..Reduction method
It is to use H2COS is reduced into H2S, the method high conversion rate, but it is of high cost and there are certain side reactions.Absorption process is to utilize alkalinity
Amine Solutions absorb acid COS gases, the method infiltration rate is fast, of low cost, but desulfuration selectivity is poor, high energy consumption,
It is primarily adapted for use in thick de-.Absorption method be using porous solid material adsorption of Low Concentration COS, make its surface of solids be enriched with and with
The process of other component separation.Common adsorbent includes activated carbon, molecular sieve, zinc oxide, iron oxide and manganese oxide etc..The method
Desulfurization depth is high, treating capacity is big but needs frequent regeneration and regeneration condition is more harsh.Oxidizing process is that COS oxidations are generated other
The sulfide easily removed tries to remove again, and flow is complex.
Hydrolyze method is first to make COS and H2O reacts, then tries the H that removing generates2The technology of S.Common COS hydrolysts
Including with γ-Al2O3And TiO2Nonmetal oxide base load for the metal oxide base carrier of representative and by representative of activated carbon
Body, have many advantages, such as room temperature activity it is high, using wide temperature range, that anti-toxicity is strong, conversion absorbs organic sulfur is efficient and save energy consumption.
The Chinese invention patent application of 106031868 A of Publication No., the patent application disclose a kind of urging for carbonyl sulfide hydrolysis
Agent and preparation method thereof and its application, prepared by infusion process using activated alumina or titanium oxide as carrier, with alkali metal,
There is good air source to fit for alkaline-earth metal or the hydrolytic catalyst of carbonyl sulfur that rare-earth oxide is active component, the catalyst
With property, sulfuric-resisting salinization ability is strong, and removal effect is good, but is not suitable for the relatively low situation of COS concentration.Publication No.
The Chinese invention patent application of 101703928 A, the patent application disclose a kind of low temperature hydrolysis carbonyl sulfur carbon base catalysts
Preparation method, the method is using activated carbon as carrier, after base extraction and activation, can remove the H generated after COS and its hydrolysis2S,
It is of low cost, but it is only applicable to the larger situation of COS concentration.Chinese invention patent of the notification number for 104667926 B, the patent
Disclose a kind of to be modified preparation methods of the γ-FeOOH as the low temperature hydrolytic catalyst of carbonyl sulfur of active component, which leads to
It crosses coprecipitation to be prepared, is applicable to CO2The higher situation of concentration, but catalytic activity need to be improved.
It is generally acknowledged that the essence of carbonyl sulfide hydrolysis reaction is base catalyzed reactions, the basic center of catalyst surface is COS water
Solve activated centre.But previous Hydrolyze method is difficult to accomplish fine de-sulfur and technological process complexity.
Invention content
The object of the present invention is to provide a kind of method that nano lamellar solid base removes carbonyl sulfur in gas, this nanometer layers
The method that the method for carbonyl sulfur is used to solve existing Hydrolyze method removing COS in shape solid base removing gas is difficult to accomplish that essence is de-
Sulphur, and the problem of technological process is complicated.
The technical solution adopted by the present invention to solve the technical problems is：Carbonyl in this nano lamellar solid base removing gas
The method of base sulphur：
Carbonyl sulfur is 40 in temperature under the effect of nano lamellar catalyzed by solid base in industrial chemicals or tail gas of sulphuroC-80oC, water
It is 1.1 with carbonyl sulfur molar ratio:1-2:1st, the material gas air speed containing COS is 1.0-4000h-1Under conditions of, water occurs
Solution and oxidation reaction, the oxidation through oxygen in water is converted into sulphur simple substance and sulfate after COS hydrolysis, realizes that COS's is de-
It removes, carbonyl sulfide removal rate is up to more than 99.5%；Nano lamellar solid base after inactivation is after soda-dip, washing, drying and roasting
Regeneration, the solid base after regeneration recycle；
The preparation method of nano lamellar metal oxide solid alkali is：Prepare Mg (NO3)2With Fe (NO3)3Solution, Mg (NO3)2With
Fe(NO3)3Solution concentration is 0.01mol/L-2.0mol/L, and Mg/Fe molar ratios are 1:4-6:1, while add M (NO3)2Into
Row metal adulterates, and M is doping metals, and M/Mg molar ratios are 1:10-5:1, hydrotalcite synthetic solvent is formed, adjusts the solution ph
To alkalinity, hydrothermal synthesis is carried out after stirring evenly, obtained solid product is washed, nano level metal doping is obtained after drying
MgFe individual layer shape hydrotalcites, obtain nano lamellar solid base after roasting.
The MgFe individual layer shape hydrotalcite synthesis conditions of nano level metal doping are in said program：100oC-280oIt is brilliant under C
Change 10h-36h, the solid matter with deionized water being centrifugally separating to obtain and ethyl alcohol wash 3-5 times, and 80oC-120 oDry 6h- under C
For 24 hours, the MgFe individual layer shape hydrotalcites of nano level metal doping are obtained.
Doping metals M is any one in Zn, Cu, Ni and Mn in said program.
The MgFe individual layer shape hydrotalcites that nano level metal adulterates in said program are 300oC-450oC roasts 3 h-12h and obtains
Nano lamellar solid base.
Hydrotalcite synthetic solvent pH value to alkaline method is adjusted in said program is：Using 0.1 mol/L-2 mol/L
KOH solution is added dropwise to hydrotalcite synthetic solvent pH value as 8.0-13.0.
The regeneration method of nano lamellar solid base is in said program：The nano lamellar solid base catalyst of inactivation is used
K2CO3, the one or both mixed solution in KOH is 20oC-80 oC impregnates 1h-24, and 3-5 extremely neutrality is washed through deionized water,
120 oC dries 1h-24h, then 300oC-450oC roasts 3h-12h, the regeneration of solid base catalyst is realized, after regeneration
Nano lamellar solid base recycles.
The invention has the advantages that：
1st, the present invention prepares metal-doped MgFe nano lamellars hydrotalcite using hydrothermal synthesis method, and nano lamellar is obtained after roasting
Oxide solid alkali, crystal size distribution range is relatively narrow, large specific surface area, and dispersion degree is high, and preparation process is simple, at low cost
It is honest and clean.
2nd, the present invention is by the hydrolysis of COS and the synergistic effect further aoxidized, and most COS is converted into elemental sulfur and sulphur at last
Hydrochlorate and remove, have higher COS removal efficiencies.
3rd, it is of the invention since sulphur simple substance and sulfate lead to its inactivation in the covering of catalyst surface, it is soaked by alkaline solution
The regeneration of catalyst can be realized in stain, washing, drying and roasting, and the catalyst after regeneration can be recycled.
4th, nano lamellar solid base is prepared in the present invention, which has larger specific surface area, dispersion degree and alkali
Property, catalysis COS hydrolysis is used it for, Applicable temperature is low, has broad application prospects, and has expanded COS hydrolyst ranges.
Description of the drawings
Fig. 1 is the evaluation result that NiMgFe oxide solids alkali removes COS；
Fig. 2 is the evaluation result that ZnMgFe oxide solids alkali removes COS；
Fig. 3 is the evaluation result that CuMgFe oxide solids alkali removes COS.
Specific embodiment
The present invention is further illustrated below in conjunction with the accompanying drawings：
Embodiment 1
Weigh 4.096g Mg (NO3)2·6H2O、2.020g Fe(NO3)3·9H2O and 1.163 g Ni (NO3)2·6H2O dissolves
It in 50 mL deionized waters and stirs evenly, n in the mixed solutionNi:nMg:nFe=4:16:5；1.0 mol/L are added dropwise
KOH is 11 to solution ph, and the mixed solution stirred evenly is transferred in reaction kettle 150oFor 24 hours, reaction terminates crystallization under C
The solid matter with deionized water being centrifugally separating to obtain and ethyl alcohol are washed 5 times respectively afterwards, 110oDry 12h, is received under C
The metal-doped NiMgFe individual layer shape hydrotalcites of meter level（Wherein Ni doping mass fractions are 26.1%）.Hydrotalcite obtained is existed
400 o8h is roasted under C and obtains nano lamellar NiMgFe solid bases.
It is 50 in reaction temperatureoC, water and carbonyl sulfur molar ratio are 1.5:1st, tail gas of sulphur containing 284 μ g/g carbonyl sulfurs
Air speed is 1000 h-1Under conditions of reacted, after testing import and export COS and H2S concentration C OS removal efficiencies are shown in Fig. 1.
By the nano lamellar NiMgFe solid base catalysts of inactivation 45oDipping 6h under C, in the KOH of 1 mol/L,
5 times are washed to after neutral through deionized water, 120oC dries 6h, then 350o8h is roasted under C, solid base catalyst can obtain
To regeneration.
Embodiment 2
Weigh 10.24g Mg (NO3)2·6H2O、4.85g Fe(NO3)3·9H2O and 2.38 g Zn (NO3)2·6H2O is dissolved in
It in 50 mL deionized waters and stirs evenly, n in the mixed solutionZn:nMg:nFe=2:10:3；0.5 mol/L KOH are added dropwise
It is 10.5 to solution ph, the mixed solution stirred evenly is transferred in reaction kettle 180oCrystallization 18h under C, reaction terminate
The solid matter with deionized water being centrifugally separating to obtain and ethyl alcohol are washed 3 times respectively afterwards, 110oDrying for 24 hours, is received under C
The metal-doped ZnMgFe individual layer shape hydrotalcites of meter level（The doping mass fraction of wherein Zn is 24.2%）.By hydrotalcite obtained
400o12 h are roasted under C and obtain nano lamellar ZnMgFe solid bases.
It is 45 in reaction temperatureoC, water and carbonyl sulfur molar ratio are 1.4:1st, the tail gas of sulphur containing 284 μ g/g carbonyl sulfurs exists
Air speed is 2400h-1Under conditions of reacted, after testing import and export COS and H2S concentration calculates COS removal efficiencies and sees Fig. 2.
By the nano lamellar ZnMgFe oxide solid base catalysts of inactivation 30oUnder C, in the K of 1mol/L2CO3Middle dipping
6h washs 5 times to after neutral, 120 through deionized wateroC dries 12h, then 400o12h, solid base catalyst are roasted under C
It is regenerated.
Embodiment 3
Weigh 20.48gMg (NO3)2·6H2O、12.12gFe(NO3)3·9H2O and 2.416g Cu (NO3)2·3H2O is dissolved in
It in 100 mL deionized waters and stirs evenly, n in the mixed solutionCu:nMg:nFe=1:8:3；Be added dropwise 1 mol/L KOH and
K2CO3Mixed solution（Wherein KOH mass fractions are 50%）It is 11 to solution ph, the mixed solution stirred evenly is transferred to instead
It answers in kettle 220oCrystallization 16h under C after reaction distinguishes the solid matter with deionized water being centrifugally separating to obtain and ethyl alcohol
Washing 5 times, 80oDrying for 24 hours, obtains the CuMgFe individual layer shape hydrotalcites of nano level metal doping under C（Wherein Cu adulterates quality
Score is 15.1%）.By hydrotalcite obtained 380o6h is roasted under C and obtains nano lamellar CuMgFe solid bases.
It is 60 in reaction temperatureoC, water and carbonyl sulfur molar ratio are 1.2:1, the tail gas of sulphur containing 284 μ g/g carbonyl sulfurs exists
Air speed is 3200h-1Under conditions of reacted, after testing import and export COS and H2S concentration calculates COS removal efficiencies and sees Fig. 3.
By the nano lamellar CuMgFe solid base catalysts of inactivation 50oDipping 12h under C, in the KOH of 2 mol/L,
5 times are washed to after neutral through deionized water, 120oC dries 12h, then 400o6h is roasted under C, solid base catalyst obtains
Regeneration.
Claims (6)
1. a kind of method of carbonyl sulfur in nano lamellar solid base removing gas, it is characterised in that：This nano lamellar solid base
The method for removing carbonyl sulfur in gas：
Carbonyl sulfur is 40 in temperature under the effect of nano lamellar catalyzed by solid base in industrial chemicals and tail gas of sulphuroC-80oC, water
It is 1.1 with carbonyl sulfur molar ratio:1-2:1st, the material gas containing COS or tail gas of sulphur air speed are 1.0-4000h-1Condition
Under, hydrolysis and oxidation reaction occurs, the oxidation through oxygen in water is converted into sulphur simple substance and sulfate after COS hydrolysis, real
The removing of existing COS, carbonyl sulfide removal rate is up to more than 99.5%；Nano lamellar solid base after inactivation is through soda-dip, washing, dry
It is regenerated after dry and roasting, the solid base after regeneration recycles；
The preparation method of nano lamellar metal oxide solid alkali is：Prepare Mg (NO3)2With Fe (NO3)3Solution, Mg (NO3)2With
Fe(NO3)3Solution concentration is 0.01mol/L-2.0mol/L, and Mg/Fe molar ratios are 1:4-6:1, while add M (NO3)2Into
Row metal adulterates, and M is doping metals, and M/Mg molar ratios are 1:10-5:1, hydrotalcite synthetic solvent is formed, adjusts the solution ph
To alkalinity, hydrothermal synthesis is carried out after stirring evenly, obtained solid product is washed, nano level metal doping is obtained after drying
MgFe individual layer shape hydrotalcites, obtain nano lamellar solid base after roasting.
2. the method for carbonyl sulfur in nano lamellar solid base removing gas according to claim 1, it is characterised in that：It is described
Nano level metal doping MgFe individual layer shape hydrotalcite synthesis conditions be：100oC-280oCrystallization 10h-36h under C, centrifugation point
3-5 times from obtained solid matter with deionized water and ethyl alcohol washing, 80oC-120 oDry 6h-24h, obtains nanometer grade gold under C
Belong to the MgFe individual layer shape hydrotalcites of doping.
3. the method for carbonyl sulfur in nano lamellar solid base removing gas according to claim 2, it is characterised in that：It is described
Doping metals M be Zn, Cu, Ni and Mn in any one.
4. the method for carbonyl sulfur in nano lamellar solid base removing gas according to claim 3, it is characterised in that：Institute
The MgFe individual layer shape hydrotalcites of nano level metal doping stated are 300oC-450oC roasts 3 h-12h and obtains nano lamellar solid
Alkali.
5. the method for carbonyl sulfur in nano lamellar solid base removing gas according to claim 4, it is characterised in that：It is described
Adjustment hydrotalcite synthetic solvent pH value to alkalinity method be：It is added dropwise using 0.1 mol/L-2 mol/L KOH solutions
It is 8.0-13.0 to hydrotalcite synthetic solvent pH value.
6. the method for carbonyl sulfur in nano lamellar solid base removing gas according to claim 5, it is characterised in that：It is described
The regeneration method of nano lamellar solid base be：The nano lamellar solid base catalyst of inactivation is used into K2CO3, one kind in KOH
Or the two mixed solution is 20oC-80 oC impregnates 1h-24,3-5 times is washed to neutrality through deionized water, 120 oC dries 1h-
For 24 hours, then 300oC-450oC roasts 3h-12h, realizes the regeneration of solid base catalyst, the nano lamellar solid base after regeneration
It recycles.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110898823A (en) * | 2019-12-10 | 2020-03-24 | 福州大学 | Magnesium aluminate spinel catalyst and application thereof in desulfurization field |
| CN116161704A (en) * | 2023-02-14 | 2023-05-26 | 苏州大学 | Doped magnesium molten iron talcum and preparation method and application thereof |
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| CN101733105A (en) * | 2009-11-27 | 2010-06-16 | 昆明理工大学 | Carbonyl sulfur hydrolyst prepared by using binary type hydrotalcite as precursor and method for preparing same |
| CN101811051A (en) * | 2009-11-24 | 2010-08-25 | 昆明理工大学 | Carbonyl sulfide hydrolysis catalyst prepared by using cobalt(Co)-nickel(Ni)-aluminum(Al) hydrotalcites as precursor and preparation method thereof |
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| CN101690893A (en) * | 2009-10-20 | 2010-04-07 | 昆明理工大学 | Carbonyl sulfide hydrolysis and preparation method thereof |
| CN101811051A (en) * | 2009-11-24 | 2010-08-25 | 昆明理工大学 | Carbonyl sulfide hydrolysis catalyst prepared by using cobalt(Co)-nickel(Ni)-aluminum(Al) hydrotalcites as precursor and preparation method thereof |
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| CN110898823B (en) * | 2019-12-10 | 2022-08-30 | 福州大学 | Magnesium aluminate spinel catalyst and application thereof in desulfurization field |
| CN116161704A (en) * | 2023-02-14 | 2023-05-26 | 苏州大学 | Doped magnesium molten iron talcum and preparation method and application thereof |
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