CN110841641A - Catalyst for preparing sulfur by selective oxidation of hydrogen sulfide and preparation method thereof - Google Patents
Catalyst for preparing sulfur by selective oxidation of hydrogen sulfide and preparation method thereof Download PDFInfo
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- CN110841641A CN110841641A CN201911160795.1A CN201911160795A CN110841641A CN 110841641 A CN110841641 A CN 110841641A CN 201911160795 A CN201911160795 A CN 201911160795A CN 110841641 A CN110841641 A CN 110841641A
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- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
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- 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
- C01B17/0434—Catalyst compositions
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- 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
- C01B17/0456—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 the hydrogen sulfide-containing gas being a Claus process tail gas
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- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The invention provides a catalyst for preparing sulfur by selective oxidation of hydrogen sulfide and a preparation method thereof. The catalyst not only has higher hydrogen sulfide conversion activity and selectivity of generating sulfur, but also has the performances of resisting sulfation, oxygen and temperature fluctuation, improves the stability and operability of the catalyst and ensures that the catalyst has longer service life.
Description
Technical Field
The invention relates to a catalyst for preparing sulfur by selective oxidation of hydrogen sulfide and a preparation method thereof, in particular to a catalyst for preparing sulfur by selective oxidation of hydrogen sulfide and a preparation method thereof, which have the advantages of higher stability, wider application range, stronger operability and longer service life.
Background
The petroleum industry, the refining of natural gas, the melting of metals in steel production, the liquefaction of coal and the like are often accompanied by the formation of considerable amounts of sulfides, mainly H2And S. It is a form of sulfide-type contaminant and also one of the sources of pollution caused by acid rain.
For high concentration of H2And S tail gas treatment, wherein a Claus tail gas recovery method is generally adopted in industry. For low concentrations of H2S (less than 15%) tail gas treatment is not economical due to the limitations of the Claus process on thermodynamics, and 3% -5% of H is still left after the Claus process treatment2S is not transformed.
The basic reaction principle of the sulfur recovery process by the direct oxidation method is as follows: h2S+O2→S+H2O + Q, which is not an equilibrium reaction, theoretically can reach 100 percent conversion rate to H in acid gas2The concentration of S has no lower limit requirement, and has the advantages of simple device, large operation flexibility, less investment, high removal rate, low consumption, easy control and operation, and the like, and is particularly suitable for treating the lean acid gas.
With the improvement of environmental protection laws and regulations and the improvement of national requirements on environmental emission standards, the direct oxidation sulfur recovery process draws high attention in the industry. The key to the process is reactor design, process optimization and catalyst development, which plays a key role.
The main problems existing in the selection of the oxidized sulfur recovery catalyst at present are as follows: (1) the selectivity of the catalyst is low, mainly the selectivity of sulfur dioxide is high, so that the recovery rate of sulfur is low; (2) the catalyst has poor stability, mainly uses raw materials which are easy to be sulfated, and has short service life although the initial activity and the low-temperature activity are higher; (3) the fluctuation of the antioxidant content is poor and only can be in O2/H2S is operated in a narrow range, which increases the difficulty of operation, or in order to realize better performance of the catalyst, the investment cost has to be increased, and the feedback regulation time is shortened; (4) is greatly influenced by temperature: process for producing sulfur by selective oxidation of hydrogen sulfideShould be strongly exothermic, especially for use in adiabatic reactors, the performance of the catalyst is more significantly affected by temperature.
Catalysts developed in the prior art can improve the yield of sulfur of the catalyst to a certain extent, for example, patent CN201710652988.3 discloses a hydrogen sulfide selective oxidation catalyst, wherein carrier raw materials comprise metatitanic acid, silica powder and calcium silicate, and iron oxide and calcium oxide are used as active components; the catalyst has high activity, is not sensitive to the influence of the steam and oxygen in the process gas, has high side pressure strength, and has high H content2The S conversion rate is high, the hydrogen sulfide conversion rate can reach more than 95%, and the sulfur yield can reach more than 90%. However, the carrier of the catalyst, such as metatitanic acid, silicon dioxide powder and calcium silicate, has poor sulfation resistance and oxygen fluctuation resistance, short service life and H2The S conversion and sulfur selectivity still can not meet the requirements.
Disclosure of Invention
The invention provides a catalyst for preparing sulfur by selective oxidation of hydrogen sulfide and a preparation method thereof. The catalyst can meet the requirement of process design on sulfur recovery, has the remarkable characteristics of strong sulfation resistance and oxidation resistance fluctuation capacity, wide application range, long service life of the catalyst and the like, can actively promote the development and popularization of a new sulfur recovery process, and has good economic benefit and environmental benefit.
The key points of the invention are as follows: the titanium-silicon composite oxide is used as a carrier of the catalyst, and compared with independent titanium oxide and silicon oxide, a chemical bond is formed between a titanium atom and a silicon atom in the titanium-silicon composite oxide, so that the performance of the catalyst is improved. The titanium-silicon composite oxide is synthesized by titanium-containing and silicon-containing salts through coprecipitation, so that the stability of the catalyst is improved, the catalyst has higher sulfation resistance and oxygen fluctuation resistance, and the service life is prolonged; and the application range of the catalyst is expanded by improving the pore structure, the specific surface area, the surface acidity and alkalinity and the like of the catalyst and matching with different auxiliaries and catalyst preparation methods.
The specific technical scheme for solving the technical key problem in the invention is as follows:
(1) a selective oxidation sulfur recovery catalyst comprising the following components: selecting titanium-silicon composite oxide as a carrier, wherein the content of the titanium-silicon composite oxide accounts for 65-90 wt%, preferably 70-85 wt% of the catalyst; selecting iron oxide or/and chromium oxide as active component, the content of which is 5-25 wt% of catalyst, preferably 10-20 wt%; the content of the active assistant is 0.5-15 wt%, preferably 1-10 wt% of the catalyst calculated by oxide.
The raw materials used by the active component are oxides, nitrates, sulfates, chlorides, carbonates and the like containing iron or/and chromium.
The raw materials used by the auxiliary agent are oxides, hydroxides, nitrates, sulfates, chlorides, carbonates, phosphates and the like of calcium, copper, sodium, zinc, magnesium, aluminum, potassium and the like.
The adhesive is sesbania powder, flour, nitric acid, etc.
Titanium-containing raw materials used for synthesizing the titanium-silicon composite oxide comprise titanium tetrachloride, titanium trichloride, titanyl sulfate, isopropyl titanate and the like, and silicon-containing raw materials comprise tetraethoxysilane, silica sol and the like; the precipitant is ammonia water, urea, sodium hydroxide, etc.
(2) The titanium-silicon composite oxide is synthesized by a precipitation method. The proportion of titanium oxide in the composite oxide is 5-95%.
The synthesis method of the titanium-silicon composite oxide comprises the following steps: dripping a precipitator into the titanium-containing and silicon-containing mixed solution, and controlling parameters such as the diameter, the specific surface area, the pore volume, the pore diameter and the like of generated precipitation particles by adjusting the pH value and the dripping speed of the solution; washing the generated precipitate, drying at 60-120 ℃, and roasting at 400-600 ℃ for 2-6h to obtain the titanium-silicon composite oxide.
(3) The preparation of the catalyst comprises the following methods:
the method comprises the following steps: uniformly mixing powder materials such as a carrier, an auxiliary agent and the like, and adding a solution containing an active component to stir and impregnate; or the soluble auxiliary agent and the active component are prepared into solution which is added into the powder material to be stirred and dipped. Aging the obtained thinner slurry or harder mud for 8-24h, drying at 80-120 ℃, crushing to 300 meshes, adding a binder for molding, and roasting at 400-600 ℃ for 2-6h to obtain the catalyst finished product.
The second method comprises the following steps: adding a carrier material into a solution containing an active component, stirring and dipping, aging the obtained thinner slurry or harder mud body for 8-24h, drying at 80-120 ℃, crushing to 300 meshes, adding a binder for forming, roasting at 400-450 ℃ for 2-6h to obtain a semi-finished product, dipping a soluble auxiliary agent, and roasting at 350-450 ℃ for 2-4h to obtain the finished catalyst.
The third method comprises the following steps: after the carrier material is added with the soluble auxiliary agent for molding, the carrier material is aged for 8-24h, dried at 40-60 ℃, roasted for 2-6h at the temperature of 400-90 ℃ to obtain a semi-finished product, the solution formed by the active components is soaked, and the finished product of the catalyst is obtained after drying at 80-100 ℃ and roasting at 350-450 ℃ for 2-4 h.
The method four comprises the following steps: the carrier material, the auxiliary agent and the active component powder are uniformly mixed, added with the binder and formed, dried at 40-60 ℃, and roasted at 400-600 ℃ for 2-6 hours to obtain the catalyst finished product.
The method five comprises the following steps: uniformly mixing the carrier material, the active component and the binder powder, adding a solution of a soluble auxiliary agent, forming, drying at 40-60 ℃, and roasting at 400-600 ℃ for 2-6 hours to obtain a catalyst finished product.
Method for preparing sulfur by selective oxidation of hydrogen sulfide, catalyst prepared by using method, and preparation method of catalyst H2The S conversion rate can reach 100/%, and the sulfur selectivity can reach more than 97/%.
Reaction conditions are as follows: space velocity of 500h-1Reaction temperature 225 ℃ and O2/H2S is 0.60, H in mixed gas before furnace2The S content is 0.75%.
Detailed Description
Detailed embodiments of the present invention will be disclosed in this section. 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. It should be understood that the detailed description of the invention is not intended to be limiting but is intended to cover all possible modifications, equivalents, and alternatives falling within the scope of the invention as defined by the appended claims. The word "may" is used throughout this application in an permissive sense rather than the mandatory sense. Similarly, unless otherwise specified, the words "include", "comprises", and "consisting of" mean "including but not limited to". The words "a" or "an" mean "at least one" and the words "a plurality" mean more than one. When abbreviations or technical terms are used, these terms are meant to have the generally accepted meaning known in the art.
This section will further illustrate the technical solutions of the present invention by combining 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:
160g of titanyl sulfate is weighed, a certain amount of water is added to completely dissolve the titanyl sulfate, 67g of silica sol containing 30 percent (wt) is added, the mixture is stirred to obtain a mixed solution, 25 percent (wt) of ammonia water solution is dripped, and the pH value of the end point is controlled to be 10-11. Standing the generated suspension for 4h, filtering and washing, drying the obtained solid at 100 ℃, roasting at 500 ℃ for 4h, and crushing to obtain the titanium-silicon composite oxide with the serial number of TS-1.
89g of titanium silicon composite oxide TS-1 is weighed, and 25g of Fe (NO) is added3)3·9H2O and 3.7g Al (NO)3)3·9H2And stirring and dipping the water solution prepared by O, aging the mud body for 12h, drying at 100 ℃, crushing, adding 2g of sesbania powder into 50g of the mud body, extruding into strips, forming, and decomposing for 4h at 500 ℃ to obtain the finished catalyst, wherein the serial number of the finished catalyst is Cat-01.
Example 2:
89g of titanium silicon composite oxide TS-1 is weighed, and 25g of Fe (NO) is added3)3·9H2And (3) stirring and dipping the solution prepared by the O, aging the mud body for 12h, drying at 100 ℃, crushing, adding 4g of sesbania powder, extruding into strips, forming, and decomposing for 4h at 500 ℃ to obtain a semi-finished catalyst. Adding 99g of the semi-finished product to 3.7g of Al (NO)3)3·9H2Soaking in water solution prepared from O in the same volume, drying at 60 ℃, and decomposing at 400 ℃ for 2h to obtain a finished catalyst product, wherein the serial number is Cat-02.
Example 3:
89g of titanium silicon composite oxide TS-1 is weighed and evenly mixed with 4g of sesbania powder, and 6.4g of Mg (NO) is added3)2·6H2And (3) extruding and forming the water solution prepared from the O, aging at normal temperature for 12h, drying at 45 ℃, and decomposing at 500 ℃ for 4h to obtain the catalyst carrier. Adding 90g of the above carrier to 25g of Fe (NO)3)3·9H2Soaking the solution prepared by O in the same volume, drying at 60 ℃, and decomposing at 400 ℃ for 2h to obtain a finished catalyst product, wherein the serial number of the finished catalyst product is Cat-03.
Example 4:
89g of titanium silicon composite oxide TS-1, 1g of nano ZnO powder and 10g of Fe are weighed2O3Mixing the powders uniformly, adding a proper amount of solution diluted by 3mL of 68% nitric acid, extruding into strips, aging at normal temperature for 12h, drying at 45 ℃, and decomposing at 500 ℃ for 4h to obtain a finished catalyst product, wherein the number of the finished catalyst product is Cat-04.
Example 5:
89g of titanium silicon composite oxide TS-1 and 10g of Fe are weighed2O3Mixing the powder with 4g sesbania powder, adding 3.7gZn (NO)3)2·6H2And (3) extruding and forming a proper amount of aqueous solution prepared from O, aging at normal temperature for 12h, drying at 45 ℃, and decomposing at 500 ℃ for 4h to obtain a catalyst finished product, wherein the catalyst finished product is numbered Cat-05.
TABLE 1 comparison of the Performance of the catalysts with the commercial samples
Catalyst evaluation conditions: space velocity of 500h-1Reaction temperature 225 ℃ and O2/H2S is 0.60, H in mixed gas before furnace2The S content is 0.75%.
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 (10)
1. A catalyst for preparing sulfur by selective oxidation of hydrogen sulfide comprises active components, wherein the active components account for 5-25 wt% of the catalyst by ferric oxide and/or chromium oxide; the content of the active auxiliary agent is 0.5-15 wt% of the catalyst calculated by oxide, and the active auxiliary agent is characterized in that: the carrier is titanium-silicon composite oxide, and the content of the titanium-silicon composite oxide accounts for 65-90 wt% of the catalyst.
2. The catalyst of claim 1, wherein: the raw materials used by the active auxiliary agent are one or more of oxides, nitrates, sulfates, chlorides and carbonates containing iron and/or chromium; the raw materials used by the auxiliary agent are one or more of oxides, hydroxides, nitrates, sulfates, chlorides, carbonates or phosphates of calcium, copper, sodium, zinc, magnesium, aluminum and potassium elements.
3. The catalyst of claim 1, wherein: the titanium-silicon composite oxide is synthesized by a precipitation method.
4. The catalyst of claim 1, wherein: the proportion of titanium oxide in the titanium-silicon composite oxide is 5-95%.
5. The catalyst of claim 3, wherein: the titanium-containing raw material used for synthesizing the titanium-silicon composite oxide is one or more of titanium tetrachloride, titanium trichloride, titanyl sulfate and isopropyl titanate, and the silicon-containing raw material used is tetraethoxysilane and/or silica sol.
6. The catalyst of claim 3, wherein: the synthesis method of the titanium-silicon composite oxide comprises the following steps: dripping a precipitator into the titanium-containing and silicon-containing mixed solution under the stirring state, and controlling the diameter, the specific surface area, the pore volume and the pore diameter of generated precipitate particles by adjusting the pH value, the dripping speed and the stirring speed of the solution; washing the generated precipitate, drying at 60-120 ℃, and roasting at 400-600 ℃ for 2-6h to obtain the titanium-silicon composite oxide.
7. The catalyst of claim 6, wherein: the precipitator is one or more of ammonia water, urea and sodium hydroxide.
8. The catalyst of claim 1, wherein: the carrier is also added with a binder, and the binder is one or more of sesbania powder, flour and nitric acid.
9. A process for the preparation of a catalyst as claimed in any one of claims 1 to 8, comprising the following steps:
the method comprises the following steps: uniformly mixing the carrier and the auxiliary agent powder material, and adding a solution containing an active component to stir and impregnate; or the soluble auxiliary agent and the active component are prepared into solution, the solution is added into the powder material of the carrier to be stirred and dipped, and the obtained thinner slurry or harder mud is aged, dried, crushed, molded and roasted to obtain the catalyst finished product;
the second method comprises the following steps: adding a carrier material into a solution containing an active component, stirring and dipping, aging, drying, crushing, forming and roasting the obtained thinner slurry or harder mud to obtain a semi-finished product, dipping a soluble auxiliary agent, and roasting to obtain a finished catalyst;
the third method comprises the following steps: adding soluble auxiliary agent into the carrier material for molding, then aging, drying and roasting to obtain a semi-finished product, dipping the semi-finished product in a solution prepared from the active components, and drying and roasting to obtain a finished catalyst product;
the method four comprises the following steps: uniformly mixing the carrier material, the auxiliary agent and the active component powder, adding a binder, forming, drying and roasting to obtain a catalyst finished product;
the method five comprises the following steps: and uniformly mixing the carrier material, the active component and the binder powder, adding a solution of a soluble auxiliary agent, forming, drying and roasting to obtain a finished catalyst.
10. A method for preparing sulfur by selective oxidation of hydrogen sulfide is characterized in that: use of the catalyst of any of claims 1 to 8, H2The S conversion rate can reach 100/%, and the sulfur selectivity can reach more than 97/%.
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| CN201911160795.1A CN110841641A (en) | 2019-11-23 | 2019-11-23 | Catalyst for preparing sulfur by selective oxidation of hydrogen sulfide and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113877623A (en) * | 2021-09-13 | 2022-01-04 | 昆明理工大学 | Preparation method and application of catalyst for purifying submerged arc furnace tail gas |
| CN114950451A (en) * | 2022-05-10 | 2022-08-30 | 中国科学院大学 | Pyrochlore composite material and preparation method and application thereof |
| CN115569649A (en) * | 2022-11-07 | 2023-01-06 | 青岛联信催化材料有限公司 | Catalyst for preparing sulfur by selective oxidation of hydrogen sulfide and preparation and use methods thereof |
-
2019
- 2019-11-23 CN CN201911160795.1A patent/CN110841641A/en not_active Withdrawn
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113877623A (en) * | 2021-09-13 | 2022-01-04 | 昆明理工大学 | Preparation method and application of catalyst for purifying submerged arc furnace tail gas |
| CN113877623B (en) * | 2021-09-13 | 2023-12-19 | 昆明理工大学 | Preparation method and application of catalyst for purifying tail gas of submerged arc furnace |
| CN114950451A (en) * | 2022-05-10 | 2022-08-30 | 中国科学院大学 | Pyrochlore composite material and preparation method and application thereof |
| CN115569649A (en) * | 2022-11-07 | 2023-01-06 | 青岛联信催化材料有限公司 | Catalyst for preparing sulfur by selective oxidation of hydrogen sulfide and preparation and use methods thereof |
| CN115569649B (en) * | 2022-11-07 | 2024-02-13 | 青岛联信催化材料有限公司 | Catalyst for preparing sulfur by selective oxidation of hydrogen sulfide and preparation and use methods thereof |
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