CN102463033A - Method for hydrolyzing carbonyl sulphide (COS) - Google Patents
Method for hydrolyzing carbonyl sulphide (COS) Download PDFInfo
- Publication number
- CN102463033A CN102463033A CN2010105518625A CN201010551862A CN102463033A CN 102463033 A CN102463033 A CN 102463033A CN 2010105518625 A CN2010105518625 A CN 2010105518625A CN 201010551862 A CN201010551862 A CN 201010551862A CN 102463033 A CN102463033 A CN 102463033A
- Authority
- CN
- China
- Prior art keywords
- cos
- catalyst
- carbonyl sulphide
- carbonyl sulfide
- earth oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- JJWKPURADFRFRB-UHFFFAOYSA-N carbonyl sulfide Chemical compound O=C=S JJWKPURADFRFRB-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 31
- 230000003301 hydrolyzing effect Effects 0.000 title abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 30
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000007062 hydrolysis Effects 0.000 claims abstract description 22
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 8
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 230000002779 inactivation Effects 0.000 abstract 1
- 229910044991 metal oxide Inorganic materials 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000009849 deactivation Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 125000001741 organic sulfur group Chemical group 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000006424 Flood reaction Methods 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Catalysts (AREA)
Abstract
The invention relates to a method for hydrolyzing carbonyl sulphide (COS), which is used for mainly solving the technical problems of narrower reaction temperature interval for COS hydrolysis, low applicative material airspeed and permanent inactivation of catalyst in the event of containing O2 in a material in the prior art. The technical problems are well solved by adopting the technical scheme as follows: the method for hydrolyzing the carbonyl sulphide comprises the step of reacting materials containing carbonyl sulphide and water in the presence of catalyst, wherein the catalyst comprises the following components in percentage by weight: (a) 1-5% of alkali carbonate, alkaline-earth metallic oxide or a mixture thereof; (b) 15-25% of rear-earth oxide in total; and (c) 70-82% of alumina. The method disclosed by the invention can be applied to industrial treatment of materials containing the carbonyl sulphide.
Description
Technical field
The present invention relates to a kind of method that is used for carbonyl sulfide hydrolysis.
Background technology
It is in the chemical process of raw material that cos (COS) method extensively is present in coal, oil, natural gas, and its existence is contaminated environment not only, and can cause catalyst poisoning in the subsequent production process, and product quality descends, equipment corrosion.Hydrolysis is to remove the most practical method of organic sulfur such as COS, and its process equation formula is: COS+H
2O → H
2S+CO
2, organic sulfur is converted into easy-to-handle H
2S is converted into S at last and reclaims.
Japan Patent JP2,002,224,572 disclose the method for a kind of cos catalyst and hydrolyzing carbonyl sulfur, and this catalyst loads on γ-Al with sodium carbonate or potash
2O
3On, the COS hydrolysising reacting temperature is 200 ℃.
U.S. Pat P4,5111,668 disclose a kind of with TiO
2Be carrier, contain a kind of alkali metal, alkaline-earth metal COS hydrolyst at least as active component, but this catalyst in use material handling COS content be merely 73ppm, and reaction temperature is higher, is 200～400 ℃.
Chinese patent CN1069673 discloses a kind of normal tempreture organic sulphur hydrolysis catalyst, and it is at spherical gamma-Al
2O
3Last load 2～5%K
2CO
3, the weak point of this catalyst is that material COS content and air speed are all lower, is respectively 1～5mg/m
3With 2,000hr
-1
Chinese patent CN1134312 discloses a kind of by 4～20wt%TiO
2And γ-Al
2O
3The organic sulfur hydrolyst of forming, the weak point of this catalyst is that air speed is merely 1,800hr
-1
Chinese patent CN1304781 discloses a kind of 83～97% γ-Al that consists of
2O
3, 2～25%K
2The COS hydrolyst of O, 0.12BaO, less than 150 ℃, COS content is less than 800mg/m in temperature
3, air speed 6,000～9,000hr
-1Carry out desulfurization under the condition, the COS hydrolysis conversion is greater than 95%.
The above-mentioned catalyst of inventing is main active component with aluminium oxide or titanium oxide all, and the weak point that is used for the COS hydrolysis with these catalyst is: the reaction temperature interval of COS hydrolysis is narrower, and the material air speed that is suitable for is low; In material, there is O
2The time, the catalyst permanent deactivation.
Summary of the invention
The technical problem that the present invention will solve is that the reaction temperature interval of the COS hydrolysis that exists in the prior art is narrow, and the material air speed that is suitable for is low, in material, has O
2The time make the problem of catalyst permanent deactivation, a kind of new method that is used for carbonyl sulfide hydrolysis is provided.It is wide that this method has the temperature range of COS hydrolysis, and the material air speed is high, and in material, have O
2The time catalyst can permanent deactivation advantage.
In order to solve the problems of the technologies described above; The technical scheme that the present invention adopts is following: a kind of method that is used for carbonyl sulfide hydrolysis; Comprise the material that contains cos and water is reacted in the presence of catalyst, wherein said catalyst comprises following component by weight percentage: (a) alkali carbonate, alkaline earth oxide or its mixture amount to 1～5%; (b) rare earth oxide amounts to 15～25%; (c) aluminium oxide 70～82%.
Preferred version is for containing cos 100～300ppm in the material described in the technique scheme, and the mol ratio preferable range of water and cos is 5～10: 1; Said reaction temperature preferable range is 50～300 ℃; The air speed preferable range of material is 5000～20000h
-1Under carry out; In the said material by weight percentage preferable range be to contain≤1% O
2
In the technique scheme, said aluminium oxide preferable range is γ-Al
2O
3Said rare earth oxide preferred version is for being selected from La
2O
3, Nd
2O
3, Sm
2O
3, Eu
2O
3Or Gd
2O
3In at least a; Said alkali carbonate, alkaline earth oxide or its mixture preferred version are selected from Na
2CO
3, K
2CO
3, at least a among MgO, CaO or the BaO.
Key problem in technology of the present invention is the component that contains rare earth oxide in the catalyst that in the hydrolytic process of COS, adopts; Because the interaction of rare earth oxide and aluminium oxide has improved activity of such catalysts; Therefore make the hydrolytic process of COS can be in wide temperature range; Carry out under the higher air speed, and within the specific limits oxygen containing material is had adaptability.The result shows that the temperature range of the inventive method is 50～300 ℃, and the material air speed can be up to 20000h
-1, and contain by weight percentage≤1% O when material
2Shi Junneng normally plays a role, and has obtained better technical effect.
The Preparation of catalysts method that adopts in the inventive method is following:
(1) chooses pulverous γ-Al
2O
3With Powdered rare earth oxide under 60～100 ℃ condition, preferred 85～95 ℃, hydrothermal treatment consists 2～8 hours, preferred 4～6 hours, process colloidal, left standstill 8～15 hours.
(2) mixture with step (1) gained was descending dry 16～24 hours at 100～130 ℃, the sample compressing tablet, fragmentation, the screening that obtain, and it is subsequent use to get its 40～60 order sample.
(3) be alkali carbonate Na with active component
2CO
3, K
2CO
3And/or at least a being distributed in the pure water of alkaline earth oxide MgO, CaO, BaO institute constitute, it is subsequent use to be configured to 10% dispersion liquid.
(4) sample with step (2) is impregnated in the dispersion liquid of step (3), floods 8～10 hours, descends dry 16～24 hours at 100～130 ℃ then, is required catalyst.
Through embodiment the present invention is done further elaboration below.
The specific embodiment
[embodiment 1]
Preparation of Catalyst: take by weighing the pulverous γ-Al of 75g respectively
2O
3With the Powdered La of 20g
2O
3, adding the 800ml deionized water, hydrothermal treatment consists is 4 hours under 85 ℃ of conditions, leaves standstill 10 hours; 110 ℃ of dryings 18 hours, get 40～60 purpose samples after compressing tablet, fragmentation, the screening then as required carrier; Take by weighing 20gNa
2CO
3Dissolve in the 180g pure water, be configured to 10% solution, the 50g solution impregnation was required catalyst in 10 hours 110 ℃ of dryings then to the 95g carrier.
The carbonyl sulfide hydrolysis technological experiment: carry out according to following technology, be reflected in Φ 10 * 300 fixed bed quartz tube reactors and carry out, temperature is 50 ℃, COS content 100ppm, H
2O: the COS mol ratio is 10: 1, air speed 5,000hr
-1, O in the material
2Weight percent content is 0.3%.Evaluation result shows that the COS conversion ratio of catalyst of the present invention is greater than 90%.
[embodiment 2～11]
Preparation of Catalyst: except the kind of concrete rare earth oxide or the concrete kind or the consumption of consumption, alkali carbonate or alkaline earth oxide; And beyond the concrete consumption of aluminium oxide changes to some extent; Catalyst preparation process is with embodiment 1, and the concrete composition of catalyst is seen table 1.
Carbonyl sulfide hydrolysis technological experiment: with O in reaction temperature, COS concentration, air speed, the material
2Content and H
2O: the COS mol ratio is a variable, and all the other are with embodiment 1, and concrete data are seen table 2.Data show that the temperature range of the inventive method is 50～300 ℃, and the material air speed can be up to 20000h
-1, and contain by weight percentage≤1% O when material
2Shi Junneng normally plays a role.
[embodiment 12]
Get the 1 prepared catalyst by embodiment, at 50-300 ℃, air speed is 10,000hr
-1, COS content is 100ppm, H
2O: the COS mol ratio is 5: 1, O in the material
2Weight percentage be that the COS conversion ratio is as shown in table 3 under 0.5% the condition, the result shows that further the inventive method has good temperature operation scope.
[embodiment 13]
Get embodiment 1 prepared catalyst, 100 ℃ of temperature, air speed is 10,000hr
-1, COS content is 150ppm, H
2O: the COS mol ratio is 5, O
2Content is under 0～1.0% condition.The result shows that further (the COS conversion ratio is as shown in table 4) the inventive method contains≤O of % in material
2Shi Junneng normally plays a role.
The composition of table 1 catalyst of the present invention
Table 2 carbonyl sulfide hydrolysis technological experiment and COS conversion ratio
Table 3 temperature is to the influence of Catalyst for CO S hydrolysing activity
| Temperature, ℃ | 50 | 100 | 150 | 200 | 250 | 300 |
| COS conversion ratio % | 91.5 | 99.2 | 99.6 | 99.9 | 99.9 | 99.7 |
O in table 4 material
2Influence to Catalyst for CO S hydrolysing activity
| O 2Content, % | 0 | 0.2 | 0.6 | 1.0 |
| COS conversion ratio % | 99.0 | 99.0 | 98.8 | 99.1 |
Claims (7)
1. method that is used for carbonyl sulfide hydrolysis; Comprise the material that contains cos and water is reacted in the presence of catalyst, wherein said catalyst comprises following component by weight percentage: (a) alkali carbonate, alkaline earth oxide or its mixture 1～5%; (b) rare earth oxide 15～25%; (c) aluminium oxide 70～82%.
2. the method for carbonyl sulfide hydrolysis according to claim 1 is characterized in that containing in the said material cos 100～300ppm; The mol ratio of water and cos is 5～10: 1.
3. the method for carbonyl sulfide hydrolysis according to claim 1 is characterized in that saidly being reflected at 50～300 ℃, and the air speed of material is 5000～20000hr
-1
4. the method for carbonyl sulfide hydrolysis according to claim 1 is characterized in that containing in the said by weight percentage material≤1% O
2
5. the method for carbonyl sulfide hydrolysis according to claim 1 is characterized in that said aluminium oxide is γ-Al
2O
3
6. the method for carbonyl sulfide hydrolysis according to claim 1 is characterized in that said rare earth oxide is for being selected from La
2O
3, Nd
2O
3, Sm
2O
3, Eu
2O
3Or Gd
2O
3In at least a.
7. the method for carbonyl sulfide hydrolysis according to claim 1 is characterized in that said alkali carbonate, alkaline earth oxide or its mixture are selected from Na
2CO
3, K
2CO
3, at least a among MgO, CaO or the BaO.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010551862.5A CN102463033B (en) | 2010-11-17 | 2010-11-17 | Method for hydrolyzing carbonyl sulphide (COS) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010551862.5A CN102463033B (en) | 2010-11-17 | 2010-11-17 | Method for hydrolyzing carbonyl sulphide (COS) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102463033A true CN102463033A (en) | 2012-05-23 |
| CN102463033B CN102463033B (en) | 2014-03-05 |
Family
ID=46067331
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010551862.5A Expired - Fee Related CN102463033B (en) | 2010-11-17 | 2010-11-17 | Method for hydrolyzing carbonyl sulphide (COS) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102463033B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105032393A (en) * | 2015-07-31 | 2015-11-11 | 青岛联信催化材料有限公司 | Organic sulfur conversion catalyst in high-pressure high-water/gas sulfur-containing raw material gas |
| CN106031868A (en) * | 2015-03-19 | 2016-10-19 | 中国石油天然气股份有限公司 | Catalyst for hydrolysis of carbonyl sulfide as well as preparation method and application thereof |
| CN111491729A (en) * | 2018-01-12 | 2020-08-04 | 三菱重工工程株式会社 | Catalyst for hydrolysis of carbonyl sulfide and method for producing same |
| CN113976101A (en) * | 2021-11-15 | 2022-01-28 | 中国科学院山西煤炭化学研究所 | Supported carbonyl sulfide hydrolysis catalyst and preparation method and application thereof |
| CN114149831A (en) * | 2021-12-08 | 2022-03-08 | 浙江三龙催化剂有限公司 | Pre-desulfurization process for blast furnace gas and application thereof |
| CN114149835A (en) * | 2021-12-08 | 2022-03-08 | 浙江三龙催化剂有限公司 | Novel deoxidation and desulfurization process and application thereof |
| CN114196449A (en) * | 2021-12-08 | 2022-03-18 | 浙江三龙催化剂有限公司 | Pre-desulfurization process for blast furnace gas and application thereof |
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|---|---|---|---|---|
| CN1304781A (en) * | 2000-07-11 | 2001-07-25 | 中国科学院山西煤炭化学研究所 | Hydrolytic catalyst of carbonyl sulfur and its preparing process and application |
| CN1403197A (en) * | 2002-09-28 | 2003-03-19 | 华东理工大学 | RE sulfide catalyst for hydrolysis of carbonyl sulfide and its prepn |
| CN1593751A (en) * | 2004-06-25 | 2005-03-16 | 同济大学 | Rare earth hydroxide catalyst for moderate/low temperature carbonyl sulfur hydrolysis and preparation method thereof |
| CN1680025A (en) * | 2005-01-19 | 2005-10-12 | 太原理工大学 | Low-temperature hydrolyst for high concentrated organosulfur and preparation thereof |
| CN101121123A (en) * | 2007-07-25 | 2008-02-13 | 太原理工大学 | Medium temperature carbon bisulfide hydrolytic catalyst and preparation method and application thereof |
-
2010
- 2010-11-17 CN CN201010551862.5A patent/CN102463033B/en not_active Expired - Fee Related
Patent Citations (5)
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| CN1304781A (en) * | 2000-07-11 | 2001-07-25 | 中国科学院山西煤炭化学研究所 | Hydrolytic catalyst of carbonyl sulfur and its preparing process and application |
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| 柯明 等: "常温羰基硫水解催化剂的进展", 《石油与天然气化工》, vol. 36, no. 4, 31 December 2007 (2007-12-31) * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106031868A (en) * | 2015-03-19 | 2016-10-19 | 中国石油天然气股份有限公司 | Catalyst for hydrolysis of carbonyl sulfide as well as preparation method and application thereof |
| CN105032393A (en) * | 2015-07-31 | 2015-11-11 | 青岛联信催化材料有限公司 | Organic sulfur conversion catalyst in high-pressure high-water/gas sulfur-containing raw material gas |
| CN105032393B (en) * | 2015-07-31 | 2018-07-13 | 青岛联信催化材料有限公司 | A kind of high water/gas Sulfur Contained Raw Gas organic sulfur conversion catalyst of high pressure |
| CN111491729A (en) * | 2018-01-12 | 2020-08-04 | 三菱重工工程株式会社 | Catalyst for hydrolysis of carbonyl sulfide and method for producing same |
| CN113976101A (en) * | 2021-11-15 | 2022-01-28 | 中国科学院山西煤炭化学研究所 | Supported carbonyl sulfide hydrolysis catalyst and preparation method and application thereof |
| CN114149831A (en) * | 2021-12-08 | 2022-03-08 | 浙江三龙催化剂有限公司 | Pre-desulfurization process for blast furnace gas and application thereof |
| CN114149835A (en) * | 2021-12-08 | 2022-03-08 | 浙江三龙催化剂有限公司 | Novel deoxidation and desulfurization process and application thereof |
| CN114196449A (en) * | 2021-12-08 | 2022-03-18 | 浙江三龙催化剂有限公司 | Pre-desulfurization process for blast furnace gas and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102463033B (en) | 2014-03-05 |
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Granted publication date: 20140305 |