CN102755886A - Preparation of vanadium intercalation hydrotalcite-like compound derivative composite oxide catalytic material and application thereof in hydrogen sulfide selective oxidation process - Google Patents
Preparation of vanadium intercalation hydrotalcite-like compound derivative composite oxide catalytic material and application thereof in hydrogen sulfide selective oxidation process Download PDFInfo
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- CN102755886A CN102755886A CN2012102401055A CN201210240105A CN102755886A CN 102755886 A CN102755886 A CN 102755886A CN 2012102401055 A CN2012102401055 A CN 2012102401055A CN 201210240105 A CN201210240105 A CN 201210240105A CN 102755886 A CN102755886 A CN 102755886A
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- vanadium
- catalytic material
- composite oxide
- hydrogen sulfide
- hydrotalcite
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Abstract
The invention relates to a preparation of a vanadium intercalation hydrotalcite-like compound derivative composite oxide catalytic material and an application of the vanadium intercalation hydrotalcite-like compound derivative composite oxide catalytic material in hydrogen sulfide selective oxidation process. The vanadium intercalation hydrotalcite-like compound derivative composite oxide catalytic material is mainly applied in hydrogen sulfide selective oxidation of acid gases in coal chemical industry and petrochemical industry to prepare elemental sulfur. The interchangeability of interlayer anions of the hydrotalcite-like compound is utilized to exchange the V10O286-ions prepared under certain pH condition to the interlayer of the hydrotalcite-like compound material, and the hydrotalcite-like compound material is calcined at a high temperature to prepare the derivative composite catalytic material. The active ingredient of the catalytic material is pentavalent vanadium ion (V5+) in vanadate (V2O86-). The catalysts have the characteristics of strong element adjustability and simple and easy preparation process, and high conversion efficiency and selectivity can be simultaneously obtained in the hydrogen sulfide selective oxidation process, so that the vanadium intercalation hydrotalcite-like compound derivative composite oxide catalytic material has a brilliant application prospect.
Description
Technical field
The present invention relates to the vanadium intercalation houghite composite oxide catalytic material (M that derives
2+ xM
3+V-LDO, x=2-4, M
2+=Mg
2+, Cu
2+, Zn
2+, Ni
2+, Co
2+, M
3+=Fe
3+, Co
3+, Al
3+, Mn
3+) preparation and reclaim the application in the process of elementary sulfur in the hydrogen sulfide selective oxidation.
Background technology
Can contain a certain amount of hydrogen sulfide gas in the acid tail gas that in Coal Chemical Industry and petroleum chemical industry production process, discharges, hydrogen sulfide is a kind of toxic and harmful with stink, and is not only harmful but also can also produce corrosiveness to production equipment to health.The increasingly stringent of the reinforcement of Along with people's environmental consciousness and environmental regulation in recent years becomes extremely urgent to the improvement of hydrogen sulfide gas.The technology of present industrial extensive use is Claus method sulfur recovery technology, and this method not only can realize the recycling of sulphur, can also effectively reduce the content of hydrogen sulfide in the tail gas, and the basic principle of this technology is following:
H
2S+(3/2)O
2→SO
2+H
2O
SO
2+2H
2S→2H
2O+(3/n)S
n
But the Claus reaction receives thermodynamics equilibrium limit, and under the condition of 3 sections Claus catalytic converters, the hydrogen sulfide conversion ratio only can reach about 97%; Still have the hydrogen sulfide gas about 3% to enter atmosphere with tail gas; For obtaining higher hydrogen sulfide conversion ratio and sulphur yield, superclaus technology is arisen at the historic moment, and its cardinal principle is to connect a reactor at claus reactor end; Be filled with hydrogen sulfide selective oxidation catalyst in this reactor, the reaction that this process takes place is mainly:
H
2S+1/2O
2→(1/n)S
n+H
2O
Because this course of reaction does not receive thermodynamic limitation, can reach 100% sulfur recovery rate in theory, therefore this reaction mainly is subject to the catalytic activity of catalyst.Recently the research to hydrogen sulfide selective oxidation catalyst mainly concentrates on molecular sieve system, carbon system etc.; And the houghite material is a kind of anionic clay materials of stratiform; It has certain soda acid position and characteristics such as interlayer anion and the cationic interchangeability of laminate; Be a kind of desirable catalyst carrier, and vanadium ion show catalytic activity preferably in the selective oxidation process of hydrogen sulfide, therefore with calcining behind the vanadium intercalation houghite; The composite oxides of deriving that enrich pore structure be can not only obtain having, and catalytic activity and sulphur selectivity preferably in hydrogen sulfide selective oxidation process, shown.
Summary of the invention
The purpose of this invention is to provide a kind of synthetic vanadium intercalation houghite composite oxide catalytic material (M that derives
2+ xM
3+V-LDO, x=2-4, M
2+=Mg
2+, Gu
2+, Zn
2+, Ni
2+, Co
2+, M
3+=Fe
3+, Co
3+, Al
3+, Mn
3+) method, and this material is applied to H in Coal Chemical Industry and the petrochemical industry sour gas
2In the selective oxidation process of S.This catalysis material has optionally characteristic of high catalytic activity and high-sulfur.
The object of the invention embodiment is following: (1) adopts the method for co-precipitation to prepare houghite (M
2+ xM
3+-LDH, x=2-4, M
2+=Mg
2+, Cu
2+, Zn
2+, Ni
2+, Co
2+, M
3+=Fe
3+, Co
3+, Al
3+, Mn
3+), a certain amount of slaine salpeter solution at 40-60 ℃, is splashed under the pH=8-10 condition in a certain amount of deionized water of inert gas (nitrogen) protection, the crystallization nucleation was 15-20 hour after titration was accomplished, and deionized water washing afterwards is centrifugal, 40-60 ℃ of oven dry down.Obtain the houghite predecessor.(2) ion-exchange prepares the vanadium intercalation houghite predecessor (M of different vanadium exchange capacities (5-20%)
2+ xM
3+V
10O
28-LDH, x=2-4, M
2+=Mg
2+, Cu
2+, Zn
2+, Ni
2+, Co
2+, M
3+=Fe
3+, Co
3+, Al
3+, Mn
3+), at first a certain amount of sodium metavanadate being dissolved in a certain amount of deionized water under the condition of pH=4.5-6, vanadium ion is with V
10O
28 6-Form exists, and then at 40-60 ℃, under the condition of pH=4.5-6, under inert gas (nitrogen) protection, this dissolving is splashed in a certain amount of houghite aqueous solution, and titration is accomplished continued and stirred 0.5-2 hour, and assurance ion-exchange is carried out fully.Suction filtration, 40-60 ℃ of oven dry obtains vanadium intercalation houghite predecessor.(3) the vanadium intercalation houghite composite oxides (M that derives
2+ xM
3+V-LDO, x=2-4, M
2+=Mg
2+, Cu
2+, Zn
2+, Ni
2+, Co
2+, M
3+=Fe
3+, Co
3+, Al
3+, Mn
3+) preparation, a certain amount of vanadium intercalation houghite predecessor is placed Muffle furnace under 500-600 ℃ of condition roasting 3-6 hour, make the composite oxides of deriving, wherein vanadium is with vanadate (V
2O
8 6-) form exist.(4) catalyst activity evaluation, wherein H
2The concentration of S is 10ppm～50000ppm; Air speed is 1000-20000h
-1O
2Concentration is H
21/2 of S concentration, nitrogen is as carrier gas.
The present invention has following beneficial effect:
1) the adjustable sex change of houghite catalysis material laminate element is strong, can prepare the composite oxide catalytic material of deriving of different elements.And the preparation process is simple and easy, be prone to realize suitability for industrialized production.
The 3 vanadium intercalation houghites composite oxide catalytic material H in Coal Chemical Industry and petrochemical industry sour gas that derives
2Use in the selective oxidation process of S, can obtain higher conversion ratio and selectivity simultaneously, thereby reach higher sulphur yield.
Description of drawings
Fig. 1: the Mg of different vanadium exchange capacities
2AlV
10O
28The X-ray diffraction spectrogram of-LDH.
Fig. 2: the Mg of 8% vanadium exchange capacity
xAlV
10O
28The X-ray diffraction spectrogram of-LDH (x=2,2.5,3,3.5,4).
Fig. 3: the Mg of different vanadium exchange capacities
2The X-ray diffraction spectrogram of AlV-LDO.
Fig. 4: the Mg of different vanadium exchange capacities
2AlV-LDO is as H
2The conversion rate curve of S selective oxidation catalyst.
Fig. 5: the Mg of different vanadium exchange capacities
2AlV-LDO is as H
2The sulphur yield curve of S selective oxidation catalyst.
The specific embodiment
Following illustrative example, explain vanadium intercalation houghite of the present invention derive composite oxide catalytic material the preparation method with its be applied to the catalytic activity and the selectivity of H2S selective oxidation process.
Embodiment 1: the vanadium intercalation magnesia-alumina hydrotalcite of different vanadium exchange capacities (5%, 8%, 10%, the 20%) composite oxides (Mg that derives
2AlV-LDO) preparation of catalysis material
The 1st step: magnalium hydrotalcite predecessor (Mg
2Al-LDH) preparation
With 30.72g Mg (NO
3)
26H
2O and 22.5gAl (NO
3)
39H
2O is dissolved in the 100mL deionized water, and magnesium ion and aluminium ion concentration are respectively 1.2moL/L and 0.6moL/L.With above-mentioned solution under 40-60 ℃, pH=8-10 condition, splash into continue to stir, in inert gas (nitrogen) the protection quantitative deionized water down, the control of pH is through dripping the NaOH solution realization of 2moL/L.Being added dropwise to complete back solution continues at 40-60 ℃, inert gas (nitrogen) protective condition stirring crystallization nucleation 15-20h down.Cooling then, centrifugal, washing are dried under the 40-60 ℃ of condition to neutral, obtain Mg
2The Al-LDH material.
The 2nd step: ion-exchange prepares the vanadium intercalation magnesia-alumina hydrotalcite predecessor (Mg of different vanadium exchange capacities (5%, 8%, 10%, 20%)
2AlV
10O
28-LDH)
The 40-60 purpose magnalium hydrotalcite material dissolves that 3g was milled is in quantitative deionized water, and this solution stirs 0.5-2h under 40-60 ℃, inert gas (nitrogen) protective condition then.0.46g sodium metavanadate (5% vanadium exchange capacity) is dissolved in the quantitative deionized water; This is dissolved in the hydrotalcite solution that is added drop-wise to stirring 0.5-2h under pH=4.5-6, inert gas (nitrogen) protective condition; The pH value of dropping process is through dripping the salpeter solution control of 0.1moL/L; Be dissolved in 40-60 ℃, inert gas (nitrogen) protective condition after being added dropwise to complete and continue to stir 0.5-2h down, cooling then, suction filtration, washing be to neutral, 40-60 ℃ of oven dry.The quality of in like manner adjusting sodium metavanadate is respectively 0.62g, 0.78g and 1.56g, makes exchange capacity and be respectively 8%, 10% and 20% precursor material (Mg
2AlV
10O
28-LDH).
The 3rd step: the vanadium intercalation magnesia-alumina hydrotalcite composite oxide material (Mg that derives
2AlV-LDO) preparation
Material in 2 is placed Muffle furnace, heat up with the speed of 10 ℃/min, roasting 3-6h under 500-600 ℃ of condition makes the vanadium intercalation magnesia-alumina hydrotalcite composite oxide material (Mg that derives
2AlV-LDO).
The vanadium intercalation magnesia-alumina hydrotalcite of the embodiment 2:8% vanadium exchange capacity composite oxides (Mg that derives
xAlV-LDO, x=2.5,3,3.5,4) preparation of catalysis material
The 1st step: magnalium hydrotalcite predecessor (Mg
xAl-LDH, x=2.5,3,3.5,4) preparation
With 30.72g Mg (NO
3)
26H
2O and 18gAl (NO
3)
39H
2O is dissolved in the quantitative deionized water, and magnesium ion and aluminium ion concentration are respectively 1.2moL/L and 0.48moL/L.With above-mentioned solution under 40-60 ℃, pH=8-10 condition, splash into continue to stir, in inert gas (nitrogen) the protection quantitative deionized water down, the control of pH is through dripping the NaOH solution realization of 2moL/L.Being added dropwise to complete back solution continues at 40-60 ℃, inert gas (nitrogen) protective condition stirring crystallization nucleation 15-20h down.Cooling then, centrifugal, washing are dried under the 40-60 ℃ of condition to neutral, obtain Mg
2.5The Al-LDH material.In like manner adjust Al (NO
3)
39H
2The quality of O is respectively 15g, 12.86g and 11.25g, makes Mg respectively
3Al-LDH, Mg
3.5Al-LDH and Mg
4The Al-LDH material.
The 2nd step: ion-exchange prepares the vanadium intercalation magnesia-alumina hydrotalcite predecessor (Mg of 8% vanadium exchange capacity
xAlV
10O
28-LDH, x=2.5,3,3.5,4)
The 40-60 purpose magnesia-alumina hydrotalcite material (Mg that 3g was milled
xAlV
10O
28-LDH, x=2.5,3,3.5,4) be dissolved in the quantitative deionized water, this solution stirs 1h under 55 ℃, nitrogen protection condition then.The 0.62g sodium metavanadate is dissolved in the quantitative deionized water; This is dissolved in the hydrotalcite solution that is added drop-wise to stirring 0.5-2h under pH=4.5-6, inert gas (nitrogen) protective condition; The pH value of dropping process is through dripping the salpeter solution control of 0.1moL/L; Be dissolved in 40-60 ℃, inert gas (nitrogen) protective condition after being added dropwise to complete and continue to stir 0.5-2h down, cooling then, suction filtration, washing be to neutral, 40-60 ℃ of oven dry.Make Mg
xAlV
10O
28-LDH, (x=2.5,3,3.5,4) material.
The 3rd step: the vanadium intercalation magnesia-alumina hydrotalcite composite oxide catalytic material (Mg that derives
xAlV-LDO, x=2.5,3,3.5,4) preparation
Method makes Mg with the step of the 3rd in the instance 1
xAlV-LDO (x=2.5,3,3.5,4) material.
Embodiment 3: the vanadium intercalation ferro-cobalt houghite of different vanadium exchange capacities (5%, 8%, 10%, the 20%) composite oxides (Mg that derives
2FeV-LDO) preparation of catalysis material
The 1st step: ferro-cobalt hydrotalcite predecessor (Mg
2Fe-LDH) preparation
With 30.72g Mg (NO
3)
26H
2O and 24.24gFe (NO
3)
39H
2O is dissolved in the quantitative deionized water, and magnesium ion and iron concentration are respectively 1.2moL/L and 0.6moL/L.With above-mentioned solution under 40-60 ℃, pH=8-10 condition, splash into continue to stir, in inert gas (nitrogen) the protection 100mL deionized water down, the control of pH is through dripping the NaOH solution realization of 2moL/L.Being added dropwise to complete back solution continues at 40-60 ℃, inert gas (nitrogen) protective condition stirring crystallization nucleation 15-20h down.Cooling then, centrifugal, washing are dried under the 40-60 ℃ of condition to neutral, obtain Mg
2The Fe-LDH material.
The 2nd step: ion-exchange prepares the vanadium intercalation ferro-cobalt houghite predecessor (Mg of different vanadium exchange capacities (5%, 8%, 10%, 20%)
2FeV
10O
28-LDH)
Method makes Mg with the step of second in the instance 1
2FeV
10O
28-LDH material.
The 3rd step: the vanadium intercalation ferro-cobalt houghite composite oxide catalytic material (Mg that derives
2FeV-LDO) preparation
Method makes Mg with the step of the 3rd in the instance 1
2The FeV-LDO material.
Embodiment 4: the Mg of different vanadium exchange capacities (5%, 8%, 10%, 20%)
2The AlV-LDO catalysis material is at H
2Catalytic activity test in the S catalytic oxidation
Fixed-bed reactor carries out H in the use laboratory
2The active testing of S catalytic oxidation, select for use an internal diameter be 10mm be about 600mm quartz ampoule as fixed bed reactors, a sand core funnel is put in the centre, with 0.6g (loadings is 2mL), size is the Mg of the different vanadium exchange capacities that prepare of 20-40m
2The AlV-LDO catalyst is put into reaction tube, service property (quality) flowmeter control flow rate of reactive gas, H
2The concentration of S is 10ppm～50000ppm; Air speed is 1000-20000h
-1O
2Concentration is H
21/2 of S concentration, nitrogen is as carrier gas.The control reaction temperature is 100 ℃～200 ℃, and reaction back gas componant and concentration use the gas-chromatography that has flame photometric detector (FPD) to detect.Pass through H in this reacting middle catalyst activity
2The conversion ratio of S and sulphur yield represent, wherein:
H
2S conversion ratio=(H in the inlet gas
2The concentration of S gas-residue H in working off one's feeling vent one's spleen
2The concentration of S gas)/inlet gas in H
2The concentration * 100% of S gas
Sulphur yield=(H in the inlet gas
2The concentration of S gas-residue H in working off one's feeling vent one's spleen
2The concentration of S gas-middle SO works off one's feeling vent one's spleen
2The concentration of gas)/inlet gas in H
2The concentration * 100% of S gas.
Claims (3)
1. the present invention relates to a kind of vanadium intercalation houghite composite oxide catalytic material (M that derives
2+ xM
3+V-LDO, x=2-4, M
2+=Mg
2+, Cu
2+, Zn
2+, Ni
2+, Co
2+, M
3+=Fe
3+, Co
3+, Al
3+, Mn
3+) reclaim the application in the process of elementary sulfur in the hydrogen sulfide selective oxidation.
2. according to claim 1, ion exchange process is under the condition of pH=4.5-6 and inert gas (nitrogen) protection, to carry out, and vanadium ion is with V under this condition
10O
28 6-Form exists, and the interlayer anion of houghite predecessor was NO after ion-exchange was accomplished
3-And/or V
10O
28 6-, the activity of such catalysts component is vanadate (V
2O
8 6-) in pentavalent vanadium ion (V
5+), vanadium ion mass exchange mark is 5%～20%.
3. according to claim 1, the intercalation of vanadium described in the present invention magnalium hydrotalcite composite oxide catalytic material of deriving is mainly used in H in Coal Chemical Industry and the petrochemical industry sour gas
2The selective oxidation process of S, suitable air speed is 1000-20000h
-1, concentration of hydrogen sulfide is 10-50000ppm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103191783A (en) * | 2013-04-18 | 2013-07-10 | 北京化工大学 | Zinc sulfide-benzoic acid nano composite photocatalytic material and preparation method thereof |
| CN108579720A (en) * | 2018-05-14 | 2018-09-28 | 福州大学 | It is a kind of using rare earth doped houghite as hydrogen sulfide selective oxidation catalyst of presoma and preparation method thereof |
| CN111545055A (en) * | 2020-06-18 | 2020-08-18 | 中国科学院大学 | Application of hydrotalcite-like compound derived composite oxide material |
| CN113351196A (en) * | 2020-03-04 | 2021-09-07 | 中国科学院生态环境研究中心 | Ceria-supported magnesium aluminum hydrotalcite material in H2Application in S selective oxidation reaction |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5514351A (en) * | 1992-04-15 | 1996-05-07 | Mobil Oil Corporation | Desulfurizing tailgas from sulfur recovery unit |
-
2012
- 2012-07-11 CN CN2012102401055A patent/CN102755886A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5514351A (en) * | 1992-04-15 | 1996-05-07 | Mobil Oil Corporation | Desulfurizing tailgas from sulfur recovery unit |
Non-Patent Citations (1)
| Title |
|---|
| 窦广玉: "V2O5/Ce--Lap和M3AlO催化剂上H2S选择性催化氧化反应过程的", 《中国科学院研究生院硕士学位论文》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103191783A (en) * | 2013-04-18 | 2013-07-10 | 北京化工大学 | Zinc sulfide-benzoic acid nano composite photocatalytic material and preparation method thereof |
| CN103191783B (en) * | 2013-04-18 | 2014-11-05 | 北京化工大学 | Zinc sulfide-benzoic acid nano composite photocatalytic material and preparation method thereof |
| CN108579720A (en) * | 2018-05-14 | 2018-09-28 | 福州大学 | It is a kind of using rare earth doped houghite as hydrogen sulfide selective oxidation catalyst of presoma and preparation method thereof |
| CN113351196A (en) * | 2020-03-04 | 2021-09-07 | 中国科学院生态环境研究中心 | Ceria-supported magnesium aluminum hydrotalcite material in H2Application in S selective oxidation reaction |
| CN111545055A (en) * | 2020-06-18 | 2020-08-18 | 中国科学院大学 | Application of hydrotalcite-like compound derived composite oxide material |
| CN111545055B (en) * | 2020-06-18 | 2022-02-11 | 中国科学院大学 | Application of hydrotalcite-like compound derived composite oxide material |
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Application publication date: 20121031 |