CN107469799B - Macroporous alumina-based catalyst suitable for pressurized sulfur recovery process and preparation method thereof - Google Patents
Macroporous alumina-based catalyst suitable for pressurized sulfur recovery process and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 73
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 26
- 239000011593 sulfur Substances 0.000 title claims abstract description 26
- 238000011084 recovery Methods 0.000 title claims abstract description 21
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims description 20
- 238000002360 preparation method Methods 0.000 title claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 14
- 229910052596 spinel Inorganic materials 0.000 claims description 14
- 229910026161 MgAl2O4 Inorganic materials 0.000 claims description 13
- 241000219782 Sesbania Species 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 9
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 239000001913 cellulose Substances 0.000 claims description 7
- 229920002678 cellulose Polymers 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 238000005096 rolling process Methods 0.000 claims description 7
- 229920002472 Starch Polymers 0.000 claims description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 6
- 239000008107 starch Substances 0.000 claims description 6
- 235000019698 starch Nutrition 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 229910003158 γ-Al2O3 Inorganic materials 0.000 claims description 5
- 239000000853 adhesive Substances 0.000 claims description 4
- 230000001070 adhesive effect Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims 1
- 239000007767 bonding agent Substances 0.000 claims 1
- 239000011148 porous material Substances 0.000 abstract description 25
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 11
- 238000009826 distribution Methods 0.000 abstract description 4
- 125000001741 organic sulfur group Chemical group 0.000 abstract description 4
- 238000009833 condensation Methods 0.000 abstract description 3
- 230000005494 condensation Effects 0.000 abstract description 3
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 230000002779 inactivation Effects 0.000 abstract description 2
- 238000011156 evaluation Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- 238000005303 weighing Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003245 coal Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910020068 MgAl Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 229910006415 θ-Al2O3 Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/02—Boron or aluminium; Oxides or hydroxides thereof
- B01J21/04—Alumina
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/64—Pore diameter
- B01J35/647—2-50 nm
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/04—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides
- C01B17/0404—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by processes comprising a dry catalytic conversion of hydrogen sulfide-containing gases, e.g. the Claus process
- C01B17/0426—Preparation of sulfur; Purification from gaseous sulfur compounds including gaseous sulfides by processes comprising a dry catalytic conversion of hydrogen sulfide-containing gases, e.g. the Claus process characterised by the catalytic conversion
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The catalyst uses an inorganic pore-forming agent to increase the macropore fraction of the catalyst, so that the catalyst has the characteristics of large average pore diameter, reasonable pore diameter distribution, good structural stability and the like, avoids pore channel blockage and even inactivation caused by the condensation of sulfur steam in catalyst pores, has high Claus reaction activity, strong organic sulfur hydrolysis performance and long service life, and is particularly suitable for a pressurized sulfur recovery process.
Description
Technical Field
The invention relates to a pressurized sulfur recovery process catalyst and a preparation method thereof, in particular to a macroporous alumina-based sulfur recovery catalyst and a preparation method thereof.
Background
At present, the domestic sulfur recovery and tail gas treatment process technology mainly adopts a Claus sulfur recovery process of high-temperature thermal reaction and two-stage catalytic reaction, the operation pressure of the process is extremely low, about 10-60 kPa, the pressure drop of the whole device is 40-50 kPa, and most of the process is filled with common alumina catalysts. Along with the continuous development of the sulfur recovery technology, in the sulfur recovery device in the coal chemical industry process, the pressurized sulfur recovery technology makes full use of the acid gas pressure of 90-120 kPa provided at the upstream, does not need a pressure reduction process, directly carries out the Claus reaction under higher pressure, has the advantages of reducing the equipment specification, reducing the occupied area of the device and the like, and is valued by the coal chemical industry. However, the process gas pressure of this technique is about 30-100kPa higher than the conventional sulfur recovery process pressure and the higher sulfur recovery process pressure results in a sulfur vapor dew point about 10-30 c higher than that of the conventional sulfur recovery process.
Typically, the inlet temperature to the claus reactor must be maintained above the minimum temperature required to prevent capillary condensation of the sulfur vapour, but to increase the conversion rate of the claus reaction, the converter is operated at as low an operating temperature as possible, thus requiring the catalyst to be operated at near the dew point of the sulfur vapour. In general, the specific surface area of a conventional alumina catalyst is about 250m2Per g, pore volume about 0.4cm3However, the average pore diameter is only about 5-10nm, the pore diameter of the catalyst is relatively small, and sulfur steam can be condensed in the catalyst pore channels under the pressurized condition to block the pore channels and even inactivate the pore channels, so that the development of a macroporous alumina-based sulfur recovery catalyst is necessary.
Disclosure of Invention
The invention provides a macroporous alumina-based sulfur recovery catalyst and a preparation method thereof, wherein the catalyst has the characteristics of large average pore diameter, reasonable pore size distribution, good structural stability and the like, avoids pore channel blockage and even inactivation caused by condensation of sulfur steam in pores of the catalyst, has high Claus reaction activity, strong organic sulfur hydrolysis performance and long service life, and is particularly suitable for a pressurized sulfur recovery process.
The specific technical scheme for solving the technical problem of the invention is as follows:
a macroporous alumina-based sulfur recovery catalyst comprises the following components: active alumina, the content of which accounts for 60 to 95 weight percent of the catalyst; the content of the pore-forming agent accounts for 5-40 wt% of the catalyst.
The pore-forming agent is inorganic or organic, wherein the inorganic pore-forming agent is gamma-Al2O3、α-Al2O3、θ-Al2O3、MgAl2O4One or more of; preferably gamma-Al2O3And/or MgAl2O4。
The organic pore-forming agent is one or a mixture of sesbania powder, cellulose, starch or polyvinyl alcohol.
The preparation method of the catalyst comprises the following steps: fully and uniformly mixing the active alumina, the inorganic pore-forming agent and the organic pore-forming agent, adding the adhesive, rolling ball forming, drying and roasting to finally obtain the macroporous alumina-based catalyst.
Wherein, the organic pore-forming agent used in the preparation process of the catalyst is one or a mixture of more than two of sesbania powder, cellulose, starch or polyvinyl alcohol, and the addition amount is 3-30 wt% of the catalyst.
Wherein the adhesive is water or dilute nitric acid.
Wherein, the calcination temperature in the catalyst preparation process is 400-800 ℃, the calcination time is 2-6h, and the preferred calcination temperature is 450-600 ℃.
The invention has the technical characteristics that: the catalyst is added with inorganic and organic pore-forming agents, can effectively enlarge the pore diameter and adjust the pore diameter distribution, and has the characteristics of large average pore diameter, reasonable pore diameter distribution, good structural stability and the like. Under the condition of pressurized sulfur recovery process, the catalyst has good Claus reaction activity and higher organic sulfur hydrolysis performance.
Detailed Description
This section will further illustrate the technical solution of the present invention by combining with detailed examples and comparative examples. The embodiments disclosed herein are examples of the present invention, which may be embodied in various forms. Therefore, specific details disclosed, including specific structural and functional details, are not intended to be limiting, but merely serve as a basis for the claims.
Example 1:
weighing 100g of pseudo-boehmite and magnesia-alumina spinel (MgAl)2O4) Mixing 10g of powder, 5g of sesbania powder and 5g of starch uniformly, mixing with 3% nitric acid solution, rolling ball forming, and roasting at 550 ℃ for 3 hours to obtain the catalyst, wherein the catalyst is numbered as Q-1. The chemical composition of the catalyst is as follows: al (Al)2O3 87.5％，MgAl2O412.5%, the strength, specific surface area and average pore diameter data of the catalyst are shown in Table 1, and the activity evaluation is shown in Table 2.
Example 2
Weighing pseudoboehmite 100g、MgAl2O420g of powder, 10g of sesbania powder and 10g of cellulose are uniformly mixed, mixed by using 3 percent nitric acid solution, formed by rolling balls and roasted at 550 ℃ for 3 hours to prepare the catalyst, wherein the serial number of the catalyst is Q-2. The chemical composition of the catalyst is as follows: al (Al)2O3 77.8％，MgAl2O422.2%, the strength, specific surface area and average pore diameter data of the catalyst are shown in Table 1, and the activity evaluation is shown in Table 2.
Example 3:
weighing 100g of pseudo-boehmite and MgAl2O4Powder 5g, gamma-Al2O310g of sesbania powder and 10g of sesbania powder are uniformly mixed, mixed with 3 percent nitric acid solution and 5 percent polyvinyl alcohol aqueous solution, and then the mixture is rolled and formed and roasted at 550 ℃ for 3 hours to obtain the catalyst, wherein the serial number of the catalyst is Q-3. The chemical composition of the catalyst is as follows: al (Al)2O3 94.1％，MgAl2O45.9%, the strength, specific surface area, average pore diameter and other data of the catalyst are shown in Table 1, and the activity evaluation is shown in Table 2.
Example 4
Weighing 100g of aluminum hydroxide and MgAl2O410g of powder, 8g of cellulose and 8g of starch are uniformly mixed, mixed with 3% nitric acid solution and 5% polyvinyl alcohol aqueous solution, and then the mixture is rolled and formed, and is roasted at 550 ℃ for 3 hours to obtain the catalyst, wherein the catalyst is numbered as Q-4. The chemical composition of the catalyst is as follows: al (Al)2O3 87.5％，MgAl2O412.5%, the strength, specific surface area, average pore diameter and other data of the catalyst are shown in Table 1, and the activity evaluation is shown in Table 2.
Example 5
The preparation of the catalyst comprises weighing 100g of aluminum hydroxide and MgAl2O4Powder 10g, gamma-Al2O320g of sesbania powder, 10g of sesbania powder and 10g of cellulose are uniformly mixed, mixed with 3 percent of nitric acid solution and 5 percent of polyvinyl alcohol aqueous solution, formed by rolling balls and roasted at 550 ℃ for 3 hours to prepare the catalyst, wherein the serial number of the catalyst is Q-5. The chemical composition of the catalyst is as follows: al (Al)2O3 90.0％，MgAl2O410.0%, the strength, specific surface area, average pore diameter and other data of the catalyst are shown in Table 1, and the activity evaluation is shown in Table 2.
Comparative example 1
Weighing 100g of pseudo-boehmite and 5g of sesbania powder, uniformly mixing, mixing with 3% nitric acid solution, rolling ball forming, and roasting at 550 ℃ for 3 hours to obtain the catalyst, wherein the serial number of the catalyst is Q-0. The chemical composition of the catalyst is as follows: al (Al)2O3100.0%, the strength, specific surface area, average pore diameter and other data of the catalyst are shown in Table 1, and the activity evaluation is shown in Table 2.
EXAMPLE 6 evaluation of catalyst Performance
Catalyst evaluation conditions:
and (3) testing the strength: randomly taking 20 samples, measuring the radial crushing strength of the catalyst on a DLII intelligent particle strength tester, and expressing the strength of the catalyst by using an average value;
claus reaction activity test: the catalyst loading is 5ml, and the space velocity is 2000h-1Water/gas 0.3, reaction pressure: 100kPa, reaction temperature: 230 ℃, 320 ℃, raw material gas (dry basis) composition: h2S 2％，SO2 1％，N2And (4) remaining;
evaluation of organic sulfur hydrolytic activity: the catalyst loading is 5ml, and the space velocity is 2000h-1Water/gas 0.3, reaction pressure: 100kPa, reaction temperature: 230 ℃, 320 ℃, raw material gas (dry basis) composition: CS2 2％，SO2 1％，N2And (4) the rest.
TABLE 1 physicochemical Properties of the catalyst
| Catalyst numbering | Strength N/particle | Specific surface m2/g | Average pore diameter nm |
| Q-1 | 134 | 255 | 15.8 |
| Q-2 | 126 | 269 | 22.7 |
| Q-3 | 141 | 274 | 28.9 |
| Q-4 | 155 | 278 | 24.6 |
| Q-5 | 174 | 261 | 32.9 |
| Q-0 | 117 | 230 | 7.8 |
| Industrial sample A | 140 | 250 | 8.5 |
Table 2 Activity evaluation data
It should be understood that the preferred embodiment processes of this example are not intended to limit the invention to the particular forms disclosed, but that the invention is to cover all modifications, equivalents, and alternatives falling within the scope of the description and defined by the appended claims.
Claims (6)
1. A macroporous alumina-based catalyst suitable for use in a pressurized sulfur recovery process, said catalyst preparation method comprising the steps of: fully and uniformly mixing active alumina, an inorganic pore-forming agent and an organic pore-forming agent, adding a bonding agent, rolling ball forming, drying and roasting to finally obtain the macroporous alumina-based catalyst;
the catalyst preparation method comprises the following components: the content of the activated alumina accounts for 60-95 wt% of the total amount of the activated alumina and the pore-forming agent; the pore-forming agent accounts for 5-40 wt% of the total amount of the activated alumina and the pore-forming agent; the method is characterized in that: the pore-forming agent is inorganic or organic; the inorganic pore-forming agent is gamma-Al 2O3 and MgAl2O4, and the organic pore-forming agent is one or a mixture of sesbania powder, cellulose, starch or polyvinyl alcohol.
2. A macroporous alumina-based catalyst suitable for use in a pressurized sulfur recovery process, said catalyst preparation method comprising the steps of: fully and uniformly mixing pseudo-boehmite and/or aluminum hydroxide, an inorganic pore-forming agent and an organic pore-forming agent, adding an adhesive, rolling ball forming, drying and roasting to finally prepare the macroporous alumina-based catalyst;
the catalyst preparation method comprises the following components: pseudo-boehmite and/or aluminum hydroxide, the content of which accounts for 60-95 wt% of the total amount of the pseudo-boehmite and/or the aluminum hydroxide and the pore-forming agent; pore-forming agent, its content is 5-4% of total quantity of pseudo-boehmite and/or aluminium hydroxide and pore-forming agent0 wt%; the method is characterized in that: the pore-forming agent is inorganic or organic; the inorganic pore-forming agent is gamma-Al2O3And MgAl2O4The organic pore-forming agent is one or a mixture of sesbania powder, cellulose, starch or polyvinyl alcohol.
3. The catalyst according to claim 1 or 2, characterized in that: the calcination temperature in the preparation method of the catalyst is 400-800 ℃, and the calcination time is 2-6 h.
4. The catalyst of claim 3, wherein: the roasting temperature is 450-600 ℃.
5. The catalyst according to claim 1 or 2, characterized in that: the adhesive is water or dilute nitric acid.
6. Use of the catalyst of claim 1 or 2 in a pressurized sulfur recovery process.
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Citations (3)
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|---|---|---|---|---|
| CN1283524A (en) * | 1999-08-04 | 2001-02-14 | 中国石化集团齐鲁石化公司 | Sulfur transform resistant macroreticular catalyst and its preparing process |
| CN103604851A (en) * | 2013-11-26 | 2014-02-26 | 武汉锆元传感技术有限公司 | Outer electrode protection layer of automobile tail gas sensor and preparation method |
| CN106348326A (en) * | 2016-08-23 | 2017-01-25 | 山东国瓷功能材料股份有限公司 | Gamma alumina, preparation method and application thereof and device |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1283524A (en) * | 1999-08-04 | 2001-02-14 | 中国石化集团齐鲁石化公司 | Sulfur transform resistant macroreticular catalyst and its preparing process |
| CN103604851A (en) * | 2013-11-26 | 2014-02-26 | 武汉锆元传感技术有限公司 | Outer electrode protection layer of automobile tail gas sensor and preparation method |
| CN106348326A (en) * | 2016-08-23 | 2017-01-25 | 山东国瓷功能材料股份有限公司 | Gamma alumina, preparation method and application thereof and device |
Non-Patent Citations (1)
| Title |
|---|
| 硫磺回收催化剂的选择及组合;廖小东等;《石油与天然气化工》;20051231;第484-488页 * |
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