CN101733105A - Carbonyl sulfur hydrolyst prepared by using binary type hydrotalcite as precursor and method for preparing same - Google Patents
Carbonyl sulfur hydrolyst prepared by using binary type hydrotalcite as precursor and method for preparing same Download PDFInfo
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- CN101733105A CN101733105A CN200910218251A CN200910218251A CN101733105A CN 101733105 A CN101733105 A CN 101733105A CN 200910218251 A CN200910218251 A CN 200910218251A CN 200910218251 A CN200910218251 A CN 200910218251A CN 101733105 A CN101733105 A CN 101733105A
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- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 8
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 8
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 8
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title abstract description 16
- 239000002243 precursor Substances 0.000 title abstract 2
- 239000003054 catalyst Substances 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000012153 distilled water Substances 0.000 claims abstract description 21
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 239000011777 magnesium Substances 0.000 claims abstract description 5
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 3
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims description 5
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 229910052717 sulfur Inorganic materials 0.000 abstract description 3
- 239000011593 sulfur Substances 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 abstract 2
- 239000007788 liquid Substances 0.000 abstract 2
- 238000009795 derivation Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 150000001455 metallic ions Chemical class 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000012716 precipitator Substances 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 238000012216 screening Methods 0.000 abstract 1
- 229910000029 sodium carbonate Inorganic materials 0.000 abstract 1
- 235000017550 sodium carbonate Nutrition 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 9
- 239000007789 gas Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 4
- 150000001450 anions Chemical class 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 150000001342 alkaline earth metals Chemical class 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 238000006477 desulfuration reaction Methods 0.000 description 2
- 230000023556 desulfurization Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 229910002651 NO3 Inorganic materials 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 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
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 125000001741 organic sulfur group Chemical group 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
- 150000003839 salts Chemical class 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
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Abstract
The invention provides a carbonyl sulfur hydrolyst prepared by using binary type hydrotalcite as a precursor and a method for preparing the same. The preparation method comprises the following steps of: at room temperature, dissolving a proper amount of nickel or magnesium and aluminum or iron in distilled water to prepare solution A, and making the mol number of the total metal reach 0.075mol, and n(M2+):n(M3+) equal to 2 to 3; dissolving 0.05mol of Na2CO3 and NaOH serving as precipitators completely reacted with binary metallic ions in the distilled water to prepare solution B; and adding the solution A into the solution B dropwise, controlling a pH value of the mixed solution to be 8 to 10 to obtain suspension liquid, crystallizing the suspension liquid in water bath at the temperature of 50 DEG C for 12 hours, and performing pumping filtration, washing by the distilled water, drying, roasting, grinding, tabletting and screening to obtain the hydrotalcite-typed derivation compound oxide catalyst. The hydrolyst prepared by the method of the invention has the advantages that: COS in the gas can be removed, simultaneously H2S generated in hydrolysis is also removed, and the sulfur removing accuracy is high; and the hydrolyst can be used at a low temperature, the operating temperature is low, and the energy consumption is saved.
Description
Technical field
The present invention relates to catalyst and preparing technical field thereof, specifically a kind of is the hydrolytic catalyst of carbonyl sulfur and the preparation method of presoma preparation with the binary type hydrotalcite, is mainly used in the cos (COS) that removes in the unstripped gas.
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.Research to the COS hydrolysis at present mainly concentrates on metal oxide such as Al
2O
3, ZrO
2, TiO
2With their mixture.
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 ℃).
CN1069673A discloses a kind of with γ-Al
2O
3Be carrier, with K
2CO
3COS hydrolyst for active component.This catalyst has hydrolysis preferably to the COS sulfides, simultaneously to H
2S also has good absorption function.
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.
Hydrotalcite (Layered Double Hydroxides, LDH) be a kind of class natural clay material with stratiform microcellular structure, has very big specific area, interlayer has tradable anion, be two hydroxy metal composite oxides that a class has the stratiform microcellular structure, (Hydrotalcite-like compounds, HTLcs) general molecular formula is [M to houghite
2+ 1-xM
x 3+(OH)
2] (A
N-)
X/nYH
2O, wherein M
2+, M
3+Represent the metal cation of divalence and trivalent respectively, A
N-For the commutative anion of interlayer, as CO
3 2-.SO
4 2-, NO
3 -Deng.LDHs has the adjustable sex change of layer structure, laminate element and the interchangeability of interlayer anion.This on chemistry and structure the special nature that shows not only make it have ion-exchange performance, but but also have an aperture modulation select shape adsoption catalysis performance, become the new material that catalytic field has the huge applications potentiality.Preparation, sign and the application of many these compounds of report had been arranged in recent years.They are comparatively stable below 400 ℃, at high temperature slough intermediary water, anion and form the composite oxides of various metals or special hydroxide, this based composite oxide has higher specific surface area and strong basicity, can be used as catalyst or carrier through after the high-temperature roasting, mainly as various base catalysts and oxidation-reduction catalyst and carrier.Alkalescence and oxidation-reduction quality by means of this based composite oxide also are used to the development environment catalyst.
It is that the nickel-base catalyst of presoma is applied to the LPG steam reforming reaction with the houghite that CN101291732A discloses a kind of, and the specific area of this catalyst and the surface area of active nickel increase, and can keep excellent catalytic activity for a long time.
CN101181686A is that precipitating reagent has synthesized ternary houghite with urea, obtains hydrocracking catalyst through 500～600 ℃ of roastings.The catalyst that this invention makes has advantages such as degree of crystallinity height, good dispersion, specific area are beaten, long service life.
Dennis E.Sparks etc. are at Applied Catalysis B:Environmental, 2008, (82): disclose among the 58-66 with coprecipitation and prepared a series of houghites, and having studied the absorption property of calcined oxide to COS, the result shows that the oxide of deriving of houghite has suction-operated preferably to COS.
According to the literature, the COS hydrolysis is a base catalyzed reactions, and the composite oxides after the houghite high-temperature roasting have higher specific surface area, decentralization and strong basicity, but the research that the composite oxides of deriving of houghite are applied to the COS hydrolysis be yet there are no report.
Summary of the invention
The purpose of this invention is to provide under a kind of cryogenic conditions with the binary type hydrotalcite is the hydrolytic catalyst of carbonyl sulfur and the preparation method of presoma preparation.This catalyst has polymolecularity, high-specific surface area, strong basicity and advantages such as normal low temperature active is good.
The present invention realizes by following method: adopt the coprecipitation that changes pH synthetic at ambient temperature, the preparation method may further comprise the steps:
(1) at room temperature with an amount of nickel, any one and aluminium in the magnesium or dissolved ferric iron in distilled water, wiring solution-forming A makes that total metal molar is 0.075mol, and n (M
2+): n (M
3+)=2～3 are with NaOH, Na
2CO
3Be precipitating reagent, get 0.05molNa
2CO
3Be dissolved in the distilled water wiring solution-forming B with NaOH with binary metal ion complete reaction;
(2) change the A solution for preparing over to separatory funnel, under room temperature and churned mechanically condition, with the speed of 3.6mL/min A solution is splashed in the B solution, it is 8～10 that control drips the terminal point pH value of solution, after dripping, still continues to stir 30min, obtains suspension at last;
(3) the suspension crystallization 12h in 50 ℃ water-bath that (2) step is obtained;
(4) product that crystallization is obtained carries out suction filtration, and makes it to be neutral with the distilled water washing.The product that obtains is put into baking oven, dry under 60 ℃ temperature;
(5) place resistance furnace at 350～650 ℃ of roasting 2h of air atmosphere step (4) products obtained therefrom, the product after the roasting through grinding, compressing tablet, sieve, get 40～60 powder materials, promptly get the houghite composite oxide catalysts of deriving.
Used metallic salt is a nitrate, and it is pure that agents useful for same is analysis.
The activity of such catalysts test is carried out in fixed bed reactors, and condition is reactor diameter 8mm, 50 ℃ of reaction temperatures, air speed 1000h
-1, COS concentration 1200mg/m
3, relative humidity 2.4%, activity is represented with COS hydrolysis clearance.
The advantage of the hydrolyst that the inventive method makes is: the COS in the gas can be removed, simultaneously the H that hydrolysis is produced
2S removes in the lump, the desulfurization precision height; Can use at low temperatures, operating temperature is low, saves energy consumption.
Description of drawings
Fig. 1 is that the cos of embodiment 1 is removed efficient variation diagram in time.
Fig. 2 is that the cos of embodiment 2 is removed efficient variation diagram in time.
Fig. 3 is that the cos of embodiment 3 is removed efficient variation diagram in time.
Fig. 4 is that the cos of embodiment 4 is removed efficient variation diagram in time.
The specific embodiment
Embodiment 1
(1) takes by weighing 12.8205gMg (NO
3)
26H
2O and 9.3782gAl (NO
3)
39H
2O is dissolved in the distilled water, and wiring solution-forming A makes that total metal molar is 0.075mol, and n (Mg
2+): n (Al
3+)=2.With NaOH, Na
2CO
3Be precipitating reagent, get 5.2995gNa
2CO
3(0.05mol) be dissolved in the distilled water wiring solution-forming B with 7gNaOH.
(2) the A solution for preparing is moved on to separatory funnel under room temperature and churned mechanically condition, with the speed of 3.6mL/min A solution is splashed in the B solution, it is 10 that control drips the terminal point pH value of solution.After dripping, still continue to stir 30min, obtain suspension at last.
(3) the suspension crystallization 12h in 50 ℃ water-bath that (2) step is obtained.
(4) product that crystallization is obtained carries out suction filtration, and makes it to be neutral with the distilled water washing.The product that obtains is put into baking oven, dry under 60 ℃ temperature.
(5) place resistance furnace at 650 ℃ of roasting 2h of air atmosphere step (4) products obtained therefrom, the product after the roasting through grinding, compressing tablet, sieve, get 40～60 powder materials, promptly get the houghite composite oxide catalysts of deriving.Active testing reaction outlet does not detect H
2S, its activity is seen Fig. 1.
Embodiment 2
(1) takes by weighing 16.3575gNi (NO
3)
26H
2O and 7.575gFe (NO
3)
39H
2O is dissolved in the distilled water, and wiring solution-forming A makes that total metal molar is 0.075mol, and n (Ni
2+): n (Fe
3+)=3.With NaOH, Na
2CO
3Be precipitating reagent, get 5.2995gNa
2CO
3(0.05mol) be dissolved in the distilled water wiring solution-forming B with 6.75gNaOH.
(2) the A solution for preparing is moved on to separatory funnel under room temperature and churned mechanically condition, with the speed of 3.6mL/min A solution is splashed in the B solution, it is 9 that control drips the terminal point pH value of solution.After dripping, still continue to stir 30min, obtain suspension at last.
(3) the suspension crystallization 12h in 50 ℃ water-bath that (2) step is obtained.
(4) product that crystallization is obtained carries out suction filtration, and makes it to be neutral with the distilled water washing.The product that obtains is put into baking oven, dry under 60 ℃ temperature.
(5) place resistance furnace at 350 ℃ of roasting 2h of air atmosphere step (4) products obtained therefrom, the product after the roasting through grinding, compressing tablet, sieve, get 40～60 powder materials, promptly get the houghite composite oxide catalysts of deriving.Active testing reaction outlet does not detect H
2S, its activity is seen Fig. 2.
Embodiment 3
(1) takes by weighing 14.4231gMg (NO
3)
26H
2O and 7.575g Fe (NO
3)
39H
2O is dissolved in the distilled water, and wiring solution-forming A makes that total metal molar is 0.075mol, and n (Mg
2+): n (Fe
3+)=3.With NaOH, Na
2CO
3Be precipitating reagent, get 5.2995gNa
2CO
3(0.05mol) be dissolved in the distilled water wiring solution-forming B with 6.75gNaOH.
(2) the A solution for preparing is transferred to separatory funnel, prepare titration.Under room temperature and churned mechanically condition, with the speed of 3.6mL/min A solution is splashed in the B solution, it is 9 that control drips the terminal point pH value of solution.After dripping, still continue to stir 30min, obtain suspension at last.
(3) the suspension crystallization 12h in 50 ℃ water-bath that (2) step is obtained.
(4) product that crystallization is obtained carries out suction filtration, and makes it to be neutral with the distilled water washing.The product that obtains is put into baking oven, dry under 60 ℃ temperature.
(5) place resistance furnace at 350 ℃ of roasting 2h of air atmosphere step (4) products obtained therefrom, the product after the roasting through grinding, compressing tablet, sieve, get 40～60 powder materials, promptly get the houghite composite oxide catalysts of deriving.Active testing reaction outlet does not detect H
2S, its activity is seen Fig. 3.
Embodiment 4
(1) takes by weighing 16.575gNi (NO
3)
26H
2O and 7.0337g Al (NO
3)
39H
2O is dissolved in the distilled water, and wiring solution-forming A makes that total metal molar is 0.075mol, and n (Ni
2+): n (Al
3+)=3.With NaOH, Na
2CO
3Be precipitating reagent, get 5.2995gNa
2CO
3(0.05mol) be dissolved in the distilled water wiring solution-forming B with 6.75gNaOH.
(2) the A solution for preparing is transferred to separatory funnel, under room temperature and churned mechanically condition, with the speed of 3.6mL/min A solution is splashed in the B solution, it is 9 that control drips the terminal point pH value of solution.After dripping, still continue to stir 30min, obtain suspension at last.
(3) the suspension crystallization 12h in 50 ℃ water-bath that (2) step is obtained.
(4) product that crystallization is obtained carries out suction filtration, and makes it to be neutral with the distilled water washing.The product that obtains is put into baking oven, dry under 60 ℃ temperature.
(5) place resistance furnace at 350 ℃ of roasting 2h of air atmosphere step (4) products obtained therefrom, the product after the roasting through grinding, compressing tablet, sieve, get 40～60 powder materials, promptly get the houghite composite oxide catalysts of deriving.Active testing reaction outlet does not detect H
2S, its activity is seen Fig. 4.
The activity of such catalysts test of above embodiment is carried out in fixed bed reactors, and condition is reactor diameter 8mm, 50 ℃ of reaction temperatures, air speed 1000h
-1, COS concentration 1200mg/m
3, relative humidity 2.4%, activity is represented with COS hydrolysis clearance.
Claims (2)
1. one kind is the preparation method of the hydrolytic catalyst of carbonyl sulfur of presoma preparation with the binary type hydrotalcite, it is characterized in that carrying out according to the following steps:
(1) at room temperature with an amount of nickel, any one and aluminium in the magnesium or dissolved ferric iron in distilled water, wiring solution-forming A makes that total metal molar is 0.075mol, and n (M
2+): n (M
3+)=2～3 are with NaOH, Na
2CO
3Be precipitating reagent, get 0.05molNa
2CO
3Be dissolved in the distilled water wiring solution-forming B with NaOH with binary metal ion complete reaction;
(2) change the A solution for preparing over to separatory funnel, under room temperature and churned mechanically condition, with the speed of 3.6mL/min A solution is splashed in the B solution, it is 8～10 that control drips the terminal point pH value of solution, after dripping, still continues to stir 30min, obtains suspension at last;
(3) the suspension crystallization 12h in 50 ℃ water-bath that (2) step is obtained;
(4) product that crystallization is obtained carries out suction filtration, and makes it to be neutral with the distilled water washing, and the product that obtains is put into baking oven, and is dry under 60 ℃ temperature;
(5) place resistance furnace at 350～650 ℃ of roasting 2h of air atmosphere step (4) products obtained therefrom, the product after the roasting through grinding, compressing tablet, sieve, get 40～60 powder materials, promptly get the houghite composite oxide catalysts of deriving.
One kind described by claim 1 be the hydrolytic catalyst of carbonyl sulfur of presoma preparation with the binary type hydrotalcite.
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| CN108246298A (en) * | 2018-02-12 | 2018-07-06 | 东北石油大学 | A kind of method of nano lamellar solid base removing carbonyl sulfur |
| CN109529795A (en) * | 2018-11-30 | 2019-03-29 | 昆明理工大学 | A kind of hydrogen sulfide adsorbent and preparation method thereof |
| CN110302789A (en) * | 2019-06-27 | 2019-10-08 | 中国科学院广州能源研究所 | A kind of Na-NiAl (O) catalyst and its application in the biological aviation fuel presoma of preparation |
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| US4810475A (en) * | 1987-08-18 | 1989-03-07 | Shell Oil Company | Removal of HCN, and HCN and COS, from a substantially chloride-free gaseous stream |
| US5360536A (en) * | 1993-08-09 | 1994-11-01 | Uop | Removal of sulfur compounds from liquid organic feedstreams |
| CN101559379A (en) * | 2009-05-22 | 2009-10-21 | 昆明理工大学 | Catalyst for hydrolyzing carbonyl sulfur and preparation method thereof |
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