CN113578329A - Hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas and preparation method thereof - Google Patents
Hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas and preparation method thereof Download PDFInfo
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- CN113578329A CN113578329A CN202110991841.3A CN202110991841A CN113578329A CN 113578329 A CN113578329 A CN 113578329A CN 202110991841 A CN202110991841 A CN 202110991841A CN 113578329 A CN113578329 A CN 113578329A
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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
- B01J23/78—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 alkali- or alkaline earth metals
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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
- B01J23/10—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of rare earths
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/002—Removal of contaminants
- C10K1/003—Removal of contaminants of acid contaminants, e.g. acid gas removal
- C10K1/004—Sulfur containing contaminants, e.g. hydrogen sulfide
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
- C10K1/00—Purifying combustible gases containing carbon monoxide
- C10K1/34—Purifying combustible gases containing carbon monoxide by catalytic conversion of impurities to more readily removable materials
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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 belongs to the technical field of industrial catalysis, and discloses a hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas and a preparation method thereof. The hydrolysis catalyst prepared by the invention comprises the following components in percentage by mass: 85-90% of carrier, 5-10% of active component and 1-3% of auxiliary agent, wherein the sum of the mass percentages of the components is 100%. Wherein, the carrier is titanium-aluminum composite oxide, the active component is one or more of ferric nitrate, cobalt nitrate, cerous nitrate and nickel nitrate, and the auxiliary agent is potassium carbonate. The hydrolysis catalyst prepared by the invention has high-efficiency catalytic hydrolysis performance on carbonyl sulfide. When the reaction temperature is 100-150 ℃, the removal rate of COS can reach more than 80 percent, and the method is suitable for low-temperature catalytic hydrolysis desulfurization of low-concentration carbonyl sulfide-containing gas such as blast furnace gas.
Description
Technical Field
The invention belongs to the technical field of industrial catalysis, and particularly relates to a hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas and a preparation method thereof.
Background
The steel industry is an important basic industry of national economy in China, provides raw material guarantee for national construction, and is a powerful support of national economy. According to the statistical data reported by the society of the iron and steel industry and the development and modification commission of China, the yields of crude steel and pig iron in China in 2019 are respectively 9.96 hundred million tons and 8.09 hundred million tons, which respectively account for 53.26 percent and 63.30 percent of the total yield of the world, which indicates that the iron and steel industry in China develops rapidly and becomes a genuine big iron and steel country. The rapid development of the steel industry in China also brings about the problems of energy consumption, environmental pollution and the like, and the research and application of the energy-saving and emission-reducing technology is a necessary measure for realizing the sustainable development of the steel industry.
The steel production in China mainly depends on a high-temperature thermal reduction mode of blast furnace ironmaking, and the total sulfur content in the byproduct blast furnace gas is about 100-200 mg/Nm3. The sulfide is mainly divided into organic sulfur and inorganic sulfur, wherein the organic sulfur is mainly carbonyl sulfide (COS). The COS can be removed by methods such as an adsorption method, a hydro-conversion method, an organic amine solvent absorption method and the like, but the methods have higher cost, are suitable for fine removal of small-gas-quantity tail gas and are not suitable for fine removal of the COS in large-gas-quantity blast furnace gas; another method is catalytic hydrolysis (COS + H)2O→H2S+CO2) Due to the mild reaction conditions, the low operation temperature and the high removal efficiency, the catalyst has become a COS conversion and removal technology widely accepted by the steel industry, wherein the selection of the catalyst is crucial to the removal effect of COS.
Currently, COS hydrolysis catalysts mainly use metal oxides such as alumina and titania as carriers to load active components and the like. However, these catalysts have high hydrolysis activity temperature and are susceptible to sulfate poisoning under the micro-oxygen atmosphere of blast furnace gas, resulting in deactivation.
Disclosure of Invention
The invention aims to solve the technical problems of low hydrolysis conversion rate, high hydrolysis temperature, poor sulfation resistance and the like in the prior art, provides a hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas and a preparation method thereof, improves the purification effect of sulfur-containing compounds in the blast furnace gas, and reduces environmental pollution.
The technical scheme adopted by the invention for solving the problems is as follows: a hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas comprises the following components in percentage by mass: 85-90% of carrier, 5-10% of active component and 1-3% of auxiliary agent, wherein the sum of the mass percentages of the components is 100%. Wherein, the carrier is titanium-aluminum composite oxide, the active component is one or more of ferric nitrate, cobalt nitrate, cerous nitrate and nickel nitrate, and the auxiliary agent is potassium carbonate.
The method for preparing the hydrolysis catalyst carrier for removing carbonyl sulfide from blast furnace gas comprises the following steps:
(1) adding a precursor of the titanium oxide and a precursor of the aluminum oxide into deionized water according to a certain molar ratio, and stirring in an ice-water bath until the titanium oxide and the aluminum oxide are completely dissolved to obtain a mixed solution;
(2) dropwise adding ammonia water into the mixed solution, stirring and adjusting the pH value to 8-10;
(3) sealing the mixture, standing and aging at room temperature for 20-30 h, and filtering out a supernatant; centrifugally washing the precipitate until the supernatant is free of chloride ions, drying the precipitate after vacuum filtration to constant weight, and grinding to obtain solid powder;
(4) and (4) calcining the solid powder obtained in the step (3) in an air atmosphere, and then mechanically tabletting, forming and sieving to obtain the titanium-aluminum composite oxide.
Furthermore, the precursor of the titanium oxide is titanium tetrachloride, and the precursor of the aluminum oxide is aluminum nitrate; the molar ratio of titanium to aluminum in the carrier is 0.5-1: 1 to 2.
The method for preparing the hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas comprises the following steps:
(1) weighing the following components in percentage by mass: 85-90% of carrier, 5-10% of active component and 1-3% of auxiliary agent, wherein the sum of the mass percentages of the components is 100%; the active component is one or more of ferric nitrate, cobalt nitrate, cerium nitrate and nickel nitrate; the auxiliary agent is potassium carbonate;
(2) preparing an active component solution: mixing 5-10% of the active component weighed in the step (1) and 1-3% of the auxiliary agent, then adding a certain amount of deionized water, and stirring until the active component and the auxiliary agent are completely dissolved;
(3) and (3) putting the carrier weighed in the step (1) into the active component solution prepared in the step (2), stirring and dipping, drying, grinding, calcining, and cooling to obtain the hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas.
Furthermore, the stirring impregnation is carried out for 1-2 h at 20-30 ℃, and then the temperature is increased to 80-90 ℃ and the stirring is carried out for 4-5 h. Magnetic stirring is adopted for stirring, and the rotating speed is 40-50 r/s; the drying is carried out for 11-13 h at the temperature of 100-120 ℃; the calcination is carried out for 5-6 h at 500-600 ℃.
Has the advantages that: the catalyst prepared by the invention has higher removal rate for carbonyl sulfide in blast furnace gas, and the addition of the transition metal oxide is beneficial to improving the sulfur poisoning resistance of the catalyst. The modified catalyst has hydrolysis conversion rate up to 80% at 100-150 deg.c. Meanwhile, the raw materials are wide in source, low in price and simple in preparation method, and can be widely applied to the steel industry.
Drawings
FIG. 1 is a graph of the desulfurization performance of the hydrolysis catalyst of the present invention.
Detailed Description
In order to facilitate understanding of the present invention, the technical solutions of the present invention are further described below with reference to the following embodiments, but the present invention is not limited thereto.
Example 1
The catalyst comprises the following raw materials: 6.044mL of titanium tetrachloride, ammonia water and 41.2643g of aluminum nitrate.
The preparation method of the carrier comprises the following steps: firstly, dissolving aluminum nitrate in 100mL of deionized water, adding titanium tetrachloride, carrying out ice-water bath and stirring vigorously until all the aluminum nitrate is dissolved to obtain a mixed solution; then dropwise adding ammonia water into the mixed solution until the pH value is 9; sealing the mixture, standing and aging at room temperature for 24 h; filtering to remove supernatant, centrifuging and washing the precipitate until no white precipitate is generated in silver nitrate titration supernatant, and then performing vacuum filtration on the mixture; drying in an oven at 105 ℃ for 12h, taking out, grinding, and calcining in a muffle furnace at 500 ℃ for 5h to obtain the titanium-aluminum composite oxide carrier with the molar ratio of titanium to aluminum being 1: 2.
Example 2
The catalyst comprises the following raw materials: 6.044mL of titanium tetrachloride, ammonia water, 41.2643g of aluminum nitrate, 3.6172g of ferric nitrate and 0.5316g of potassium carbonate.
The support preparation procedure was the same as in example 1, and the catalyst preparation method included: firstly, calcining a titanium-aluminum composite oxide carrier to remove impurities for later use; secondly, dissolving the titanium-aluminum composite oxide carrier in 50mL of deionized water, and adding ferric nitrate and potassium carbonate; uniformly stirring at 45r/s for 2h under magnetic stirring at 25 ℃, heating to 85 ℃, continuously stirring and impregnating at 45r/s, drying in an oven at 105 ℃ for 12h after water is evaporated to dryness, taking out, grinding, and calcining in a muffle furnace at 500 ℃ for 5h to obtain the final product with the component mass fraction K3Fe5TiAl hydrolysis catalyst.
Example 3
The preparation procedure was the same as in example 2, except that the catalyst starting materials were: 6.044mL of titanium tetrachloride, ammonia water, 41.2643g of aluminum nitrate, 2.4691g of cobalt nitrate and 0.5316g of potassium carbonate.
The prepared catalyst has the mass fraction of K3Co5TiAl hydrolysis catalyst.
Example 4
The preparation procedure was the same as in example 2, except that the catalyst starting materials were: 6.044mL of titanium tetrachloride, ammonia water, 41.2643g of aluminum nitrate, 1.5493g of cerium nitrate and 0.5316g of potassium carbonate.
The prepared catalyst has the mass fraction of K3Ce5TiAl hydrolysis catalyst.
Example 5
The preparation procedure was the same as in example 2, except that the catalyst starting materials were: 6.044mL of titanium tetrachloride, ammonia water, 41.2643g of aluminum nitrate, 2.4775g of nickel nitrate and 0.5316g of potassium carbonate.
The prepared catalyst has the mass fraction of K3Ni5TiAl hydrolysis catalyst.
The catalysts obtained in examples 2 to 5 were analyzed and tested, the activity and stability results of the catalysts were expressed as COS removal rate, and the COS concentration was measured by on-line gas chromatography. Test conditionsComprises the following steps: and (3) carrying out activity test of COS catalytic hydrolysis in a fixed bed quartz tube reactor, wherein the loading amount of the catalyst is 0.5mL, the granularity is 40-60 meshes, the reaction temperature is 50-150 ℃, each reaction temperature is continuously detected for 2h, and the test temperature points are separated by 25 ℃. The concentration of COS in the feed gas is 200mg/m3，N2The total smoke gas is 200mL/min as balance gas; the gases are gradually mixed by a mass flow meter, then added with water vapor by a water saturator and finally enter an air mixer for full mixing; the reactor is a quartz tube with the inner diameter of 10mm, and a vertical tube type heating furnace with a temperature control system provides a reaction temperature environment.
As can be seen from FIG. 1, the hydrolysis catalyst prepared by the invention has a good removal effect on COS, and can realize a removal rate of COS of more than 80% at 100-150 ℃.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (12)
1. A hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas is characterized by comprising the following components in percentage by mass: 85-90% of carrier, 5-10% of active component and 1-3% of auxiliary agent, wherein the sum of the mass percentages of the components is 100%.
2. The hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas according to claim 1, wherein the carrier is a titanium-aluminum composite oxide.
3. A method for preparing the titanium-aluminum composite oxide support according to claim 2, which is carried out specifically according to the following steps:
1) adding a precursor of the titanium oxide and a precursor of the aluminum oxide into deionized water according to a certain molar ratio, and stirring in an ice-water bath until the titanium oxide and the aluminum oxide are completely dissolved to obtain a mixed solution;
2) dropwise adding ammonia water into the mixed solution, stirring and adjusting the pH value to 8-10;
3) sealing the mixture, standing and aging at room temperature for 24 hours, and filtering out the supernatant; centrifugally washing the precipitate until the supernatant is free of chloride ions, drying the precipitate after vacuum filtration to constant weight, and grinding to obtain solid powder;
4) calcining the solid powder obtained in the step 3) in the air atmosphere, and then mechanically tabletting, forming and sieving to obtain the titanium-aluminum composite oxide.
4. The method for producing a titanium-aluminum composite oxide support according to claim 3, characterized in that: in the step 1), the precursor of the titanium oxide is titanium tetrachloride, and the precursor of the aluminum oxide is aluminum nitrate; wherein the molar ratio of titanium to aluminum in the carrier is 0.5-1: 1 to 2.
5. The hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas according to claim 1, wherein the active component is one or more of ferric nitrate, cobalt nitrate, cerium nitrate and nickel nitrate.
6. The hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas according to claim 1, wherein the assistant is potassium carbonate.
7. A preparation method of a hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas is characterized by comprising the following steps:
1) weighing the following components in percentage by mass: 85-90% of carrier, 5-10% of active component and 1-3% of auxiliary agent, wherein the sum of the mass percentages of the components is 100%; the active component is one or more of ferric nitrate, cobalt nitrate, cerium nitrate and nickel nitrate; the auxiliary agent is potassium carbonate;
2) preparing an active component solution: mixing 5-10% of the active component weighed in the step 1) and 1-3% of the auxiliary agent, then adding a certain amount of deionized water, and stirring until the active component and the auxiliary agent are completely dissolved;
3) putting the carrier weighed in the step 1) into the active component solution prepared in the step 2), stirring and dipping, drying, grinding, calcining, and cooling to obtain the hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas.
8. The method for preparing the hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas according to claim 7, wherein the hydrolysis catalyst comprises: in the step 3), stirring and dipping are carried out for 1-2 h at 20-30 ℃, and then the temperature is increased to 80-90 ℃ and stirring is carried out for 4-5 h.
9. The preparation method of the hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas according to claim 8, wherein the stirring is magnetic stirring with a rotating speed of 40-50 r/s.
10. The preparation method of the hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas according to claim 3 or 7, wherein the drying is performed at 100-120 ℃ for 11-13 h.
11. The preparation method of the hydrolysis catalyst for removing carbonyl sulfide in blast furnace gas according to claim 3 or 7, wherein the calcining is performed at 500-600 ℃ for 5-6 h.
12. The hydrolysis catalyst for removing carbonyl sulfide from blast furnace gas, which is prepared by the method of claims 1-11.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN114196448A (en) * | 2022-02-16 | 2022-03-18 | 北京中航天业科技有限公司 | Full-flow dry type blast furnace gas fine desulfurization system and method |
| 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 |
| CN114367279A (en) * | 2021-12-31 | 2022-04-19 | 东南大学 | Low-temperature poisoning-resistant hydrolysis catalyst for fine desulfurization of blast furnace gas and preparation method thereof |
| CN114522691A (en) * | 2022-02-21 | 2022-05-24 | 福州大学 | Preparation method of composite metal oxide for organic sulfur catalytic hydrolysis |
| CN115445602A (en) * | 2022-08-31 | 2022-12-09 | 盐城市兰丰环境工程科技有限公司 | Catalyst for organic sulfur hydrolysis of blast furnace gas and preparation and application methods thereof |
| CN115672367A (en) * | 2022-10-31 | 2023-02-03 | 触媒净化技术(南京)有限公司 | Glass fiber corrugated plate type blast furnace gas carbonyl sulfide hydrolysis catalyst and preparation method thereof |
| CN116020434A (en) * | 2023-02-15 | 2023-04-28 | 北京中航天业科技有限公司 | Sulfur accumulation-free and deactivation-resistant carbonyl sulfide hydrolysis catalyst and application thereof |
| CN117563631A (en) * | 2024-01-16 | 2024-02-20 | 陕西驭腾化学控股发展有限公司 | Titanium dioxide-silicon dioxide aerogel catalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| CN114367279A (en) * | 2021-12-31 | 2022-04-19 | 东南大学 | Low-temperature poisoning-resistant hydrolysis catalyst for fine desulfurization of blast furnace gas and preparation method thereof |
| CN114196448A (en) * | 2022-02-16 | 2022-03-18 | 北京中航天业科技有限公司 | Full-flow dry type blast furnace gas fine desulfurization system and method |
| CN114522691B (en) * | 2022-02-21 | 2023-05-30 | 福州大学 | Preparation method of composite metal oxide for organic sulfur catalytic hydrolysis |
| CN114522691A (en) * | 2022-02-21 | 2022-05-24 | 福州大学 | Preparation method of composite metal oxide for organic sulfur catalytic hydrolysis |
| CN115445602A (en) * | 2022-08-31 | 2022-12-09 | 盐城市兰丰环境工程科技有限公司 | Catalyst for organic sulfur hydrolysis of blast furnace gas and preparation and application methods thereof |
| CN115445602B (en) * | 2022-08-31 | 2023-09-26 | 盐城市兰丰环境工程科技有限公司 | Catalyst for hydrolyzing organic sulfur in blast furnace gas and preparation and application methods thereof |
| CN115672367A (en) * | 2022-10-31 | 2023-02-03 | 触媒净化技术(南京)有限公司 | Glass fiber corrugated plate type blast furnace gas carbonyl sulfide hydrolysis catalyst and preparation method thereof |
| CN116020434A (en) * | 2023-02-15 | 2023-04-28 | 北京中航天业科技有限公司 | Sulfur accumulation-free and deactivation-resistant carbonyl sulfide hydrolysis catalyst and application thereof |
| CN117563631A (en) * | 2024-01-16 | 2024-02-20 | 陕西驭腾化学控股发展有限公司 | Titanium dioxide-silicon dioxide aerogel catalyst and preparation method and application thereof |
| CN117563631B (en) * | 2024-01-16 | 2024-03-26 | 陕西驭腾化学控股发展有限公司 | Hydrolysis catalyst for blast furnace gas fine desulfurization, preparation method and application |
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