CN111592474A - Preparation method of complex iron catalyst for wet desulphurization - Google Patents
Preparation method of complex iron catalyst for wet desulphurization Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/04—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing carboxylic acids or their salts
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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
- B01J33/00—Protection of catalysts, e.g. by coating
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
- C10L3/102—Removal of contaminants of acid contaminants
- C10L3/103—Sulfur containing contaminants
Abstract
The invention discloses a preparation method of a complex iron catalyst for wet desulphurization, belonging to the technical field of environmental protection. The preparation method comprises the following steps: the method comprises the following steps: (1) preparing sulfophthalic acid; (2) sulfophthalic acid reacts with sodium hydroxide to prepare a compound I; (3) reacting the compound I with cobalt chloride to prepare a compound II; (4) reacting the compound I with an iron-containing compound to prepare a compound III; (5) reacting the compound II with a compound III to obtain a compound IV; (6) and (3) preparing a stabilizer, (7) uniformly mixing the compound IV with a bistable agent, heating, cooling and drying to obtain the catalyst. The composite iron catalyst for sulfur-containing gas desulfurization prepared by the invention greatly improves the working sulfur capacity, reduces the concentration of iron ions while completing the absorption of hydrogen sulfide, achieves an ideal absorption effect, reduces the occurrence probability of side reactions, can achieve a good effect of absorbing hydrogen sulfide, and can inhibit the generation of side salts.
Description
Technical Field
The invention relates to a desulfurization catalyst, in particular to a complex iron catalyst, and belongs to the technical field of environmental protection.
Background
Chemical raw material gas which takes coal, natural gas and the like as raw materials and other exhaust gas contain a certain amount of sulfide, and if the sulfide is not removed, serious air pollution is formed. In use, hydrogen sulfide can cause corrosion of equipment and piping and catalyst poisoning, leading to increased production costs and affecting product quality. Therefore, the gas must be subjected to a desulfurization treatment before being used for fuel gas and synthesis gas. There are many methods for desulfurizing gas, and they can be classified into dry desulfurization and wet desulfurization according to the state of the desulfurizing agent. The dry desulfurization process utilizes the solid adsorbent to remove the hydrogen sulfide and organic sulfur in the coal gas, has higher desulfurization purification degree, is suitable for the treatment of low-sulfur gas and is mainly used for fine desulfurization. Wet desulfurization can be classified into a chemical absorption method, a physical absorption method and a physical-chemical absorption method according to the absorption and regeneration properties of desulfurization solutions. The chemical absorption method is divided into a neutralization method and a wet oxidation method, and the main principle is that the existing form of sulfur is changed through a chemical reaction. The physical absorption method adopts organic solvent as absorbent to absorb H under pressure2S, reducing the pressure to absorb H2S is released, and the absorbent is recycled. In large-scale projects, the primary desulfurization of chemical raw material gas mainly adopts wet desulfurization.
Chinese patent 201610777813.0 discloses a complex iron desulfurization solution for wet desulfurization and a preparation method thereof, wherein the complex iron desulfurization solution comprises an antioxidant, a nonionic surfactant, a defoaming agent, a complex iron catalyst and water, and the preparation method has the disadvantages of complex process and poor stability.
Chinese patent CN1398659A discloses a biochemical iron-alkali solution catalytic method for desulfurizing gas, which adopts an iron-alkali solution to remove organic sulfur and/or inorganic sulfur in cold flow gas, the iron-alkali solution is prepared by aerobic bacteria spores and/or aerobic bacteria, an iron compound, an alkaline substance, a phenolic substance and water, and is a biochemical wet desulfurization technology, but the catalyst has high cost and poor stability, and the investment in the early stage in practical application is large.
Document ISS complex iron-polyphenol catalyst desulfurization technology discloses a complex iron-polyphenol desulfurization catalyst, the main active components are complex iron compound and polyphenol substance, the complex of variable valence metal iron is used as desulfurization catalyst, the polyphenol substance is used as regeneration catalyst, organic sulfur is firstly absorbed and converted in the desulfurization process, and then oxidized into elemental sulfur by the catalyst to be removed, but a large amount of side reactions are generated in the desulfurization and regeneration processes.
Traditional iron catalyst all has the corrosivity strong, the desulfurization is with high costs and the shortcoming that the sulfur capacity is low to iron ion degradation speed is fast, and the poor stability deposits much, uses for a long time and easily causes desulfurization system suspended solid to increase and blocks up the filler, and the corrosion of equipment pipeline aggravation brings the hidden danger for the continuity and the operability of production.
Disclosure of Invention
Aiming at the technical problems in the prior art, the technical problem to be solved by the invention is to provide a preparation method of a complex iron catalyst for wet desulphurization, the prepared complex iron catalyst for desulphurization of sulfur-containing gas greatly improves the working sulfur capacity, reduces the stability of iron ions in a system while completing the absorption of hydrogen sulfide, achieves an ideal absorption effect, reduces the occurrence probability of side reactions, can achieve a good effect of absorbing hydrogen sulfide, and can inhibit the generation of side salts.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of a complex iron catalyst for wet desulphurization comprises the following steps: (1) adding phthalic anhydride and fuming sulfuric acid into a reaction kettle, heating to 200-240 ℃ until the reaction is completed, and obtaining sulfophthalic acid; (2) adding sodium hydroxide into sulfophthalic acid, and stirring until the reaction is completed to obtain a compound I; (3) heating the compound I and cobalt chloride to 200-240 ℃ for reaction to obtain a compound II; (4) heating the compound I and an iron-containing compound to 200-240 ℃ for reaction to obtain a compound III; (5) heating the compound II and the compound III to 240-280 ℃ for reaction to obtain a compound IV; (6) preparing a stabilizer: uniformly mixing ATMP, water, ammonia water and citric acid to prepare a bistable agent; (7) and (3) uniformly mixing the compound IV and a bistable agent, heating to 80 ℃, keeping the temperature constant for one hour, cooling and drying to obtain the catalyst.
The mass ratio of the phthalic anhydride to the fuming sulfuric acid is 1-2: 1.
The mass ratio of ATMP, water, ammonia water and citric acid is 1:1-5:0.05-0.15: 0.05-0.15.
The preferred mass ratio of ATMP, water, ammonia water and citric acid is 1:3:0.1: 0.1.
The mass ratio of the compound IV to the bistable agent is 2-5: 1.
The mass ratio of the compound IV to the bistable agent is 3: 1.
The iron-containing compound is ferric hydroxide or ferric chloride.
Phthalic anhydride is short for phthalic anhydride, and has a structural formula as follows:
ATMP is aminotrimethylene phosphonic acid
The structural formula of the sulfophthalic acid is
The structural formula of the compound I is
The structural formula of the compound II is
The structural formula of the compound III is
The structural formula of the compound IV is
The bi-stabilizing agent can effectively reduce the occurrence of free radicals of iron ions and prevent precipitation.
The invention has the beneficial effects that:
the invention utilizes the oxygen carrying and carrying of the valence-variable iron ions and the cobalt ions, reduces the concentration of the iron ions while completing the absorption of the hydrogen sulfide, achieves the ideal absorption effect and controls the generation of side reactions.
The novel composite catalyst is synthesized by adopting the preparation of iron-cobalt macromolecular substances and a stabilizer. The precipitation of iron ions is effectively controlled, the working sulfur capacity is improved due to the strong oxygen carrying and carrying capacity of cobalt ions in the using process, the sulfur capacity of the catalyst can reach 0.2 percent, the concentration of the iron ions in the solution is reduced, the catalyst is 1/3 of the concentration of the iron ions of the traditional complex iron catalyst, the effect of absorbing hydrogen sulfide can be achieved well, and the generation of secondary salt is inhibited.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The preparation method of the complex iron catalyst for wet desulphurization comprises the following steps:
(1) adding phthalic anhydride and fuming sulfuric acid with the mass ratio of 1.5:1 into a reaction kettle, heating to 240 ℃ until the reaction is completed, and obtaining sulfophthalic acid;
(2) adding sodium hydroxide into sulfophthalic acid, and stirring until the reaction is completed to obtain a compound I;
(3) heating a compound I and cobalt chloride in a molar ratio of 1:2 to 220 ℃ for reaction to obtain a compound II;
(4) heating a compound I and ferric hydroxide in a molar ratio of 1:2 to 220 ℃ for reaction to obtain a compound III;
(5) heating a compound II and a compound III in a molar ratio of 1:1 to 260 ℃ for reaction to obtain a compound IV;
(6) preparing a stabilizer: uniformly mixing ATMP, water, ammonia water and citric acid in a mass ratio of 1:3:0.1:0.1 to prepare a bistable agent;
(7) and (3) uniformly mixing the compound IV with the bistable agent in a mass ratio of 3:1, heating to 80 ℃, keeping the temperature constant for one hour, cooling and drying to obtain the catalyst.
Example 2
The preparation method of the complex iron catalyst for wet desulphurization comprises the following steps:
(1) adding phthalic anhydride and fuming sulfuric acid in a mass ratio of 1:1 into a reaction kettle, heating to 220 ℃ until the reaction is complete, and obtaining sulfophthalic acid;
(2) adding sodium hydroxide into sulfophthalic acid, and stirring until the reaction is completed to obtain a compound I;
(3) heating a compound I and cobalt chloride in a molar ratio of 1:2 to react at 200 ℃ to obtain a compound II;
(4) heating a compound I and ferric hydroxide in a molar ratio of 1:2 to 240 ℃ for reaction to obtain a compound III;
(5) heating a compound II and a compound III in a molar ratio of 1:1 to 280 ℃ to react to obtain a compound IV;
(6) preparing a stabilizer: uniformly mixing ATMP, water, ammonia water and citric acid in a mass ratio of 1:5:0.05:0.05 to prepare a bistable agent;
(7) and (3) uniformly mixing the compound IV with the bistable agent in the mass ratio of 2:1, heating to 80 ℃, keeping the temperature constant for one hour, cooling and drying to obtain the catalyst.
Example 3
The preparation method of the complex iron catalyst for wet desulphurization comprises the following steps:
(1) adding phthalic anhydride and fuming sulfuric acid in a mass ratio of 2:1 into a reaction kettle, heating to 240 ℃ until the reaction is complete, and obtaining sulfophthalic acid;
(2) adding sodium hydroxide into sulfophthalic acid, and stirring until the reaction is completed to obtain a compound I;
(3) heating a compound I and cobalt chloride in a molar ratio of 1:2 to 240 ℃ for reaction to obtain a compound II;
(4) heating a compound I and ferric hydroxide in a molar ratio of 1:2 to 200 ℃ for reaction to obtain a compound III;
(5) heating a compound II and a compound III in a molar ratio of 1:1 to 240 ℃ for reaction to obtain a compound IV;
(6) preparing a stabilizer: uniformly mixing ATMP, water, ammonia water and citric acid in a mass ratio of 1:1:0.15:0.1 to prepare a bistable agent;
(7) and (3) uniformly mixing the compound IV with the bistable agent in a mass ratio of 5:1, heating to 80 ℃, keeping the temperature constant for one hour, cooling and drying to obtain the catalyst.
Example 4
The preparation method of the complex iron catalyst for wet desulphurization comprises the following steps:
(1) adding phthalic anhydride and fuming sulfuric acid with the mass ratio of 1.5:1 into a reaction kettle, heating to 240 ℃ until the reaction is completed, and obtaining sulfophthalic acid;
(2) adding sodium hydroxide into sulfophthalic acid, and stirring until the reaction is completed to obtain a compound I;
(3) heating a compound I and cobalt chloride in a molar ratio of 1:2 to react at 200 ℃ to obtain a compound II;
(4) heating a compound I and ferric hydroxide in a molar ratio of 1:2 to 210 ℃ for reaction to obtain a compound III;
(5) heating a compound II and a compound III in a molar ratio of 1:1 to 260 ℃ for reaction to obtain a compound IV;
(6) preparing a stabilizer: uniformly mixing ATMP, water, ammonia water and citric acid in a mass ratio of 1:5:0.05:0.1 to prepare a bistable agent;
(7) and (3) uniformly mixing the compound IV with the bistable agent in a mass ratio of 4:1, heating to 80 ℃, keeping the temperature constant for one hour, cooling and drying to obtain the catalyst.
Example 5
The preparation method of the complex iron catalyst for wet desulphurization comprises the following steps:
(1) adding phthalic anhydride and fuming sulfuric acid with the mass ratio of 1.5:1 into a reaction kettle, heating to 240 ℃ until the reaction is completed, and obtaining sulfophthalic acid;
(2) adding sodium hydroxide into sulfophthalic acid, and stirring until the reaction is completed to obtain a compound I;
(3) heating a compound I and cobalt chloride in a molar ratio of 1:2 to 210 ℃ for reaction to obtain a compound II;
(4) heating a compound I and ferric hydroxide in a molar ratio of 1:2 to 240 ℃ for reaction to obtain a compound III;
(5) heating a compound II and a compound III in a molar ratio of 1:1 to 280 ℃ to react to obtain a compound IV;
(6) preparing a stabilizer: uniformly mixing ATMP, water, ammonia water and citric acid in a mass ratio of 1:4:0.1:0.1 to prepare a bistable agent;
(7) and (3) uniformly mixing the compound IV with the bistable agent in a mass ratio of 3:1, heating to 80 ℃, keeping the temperature constant for one hour, cooling and drying to obtain the catalyst.
Use case one: coke oven gas desulfurization
The using time is 2019, 12 months and 3 months.
Coke oven gas yield: 35000Nm3H hydrogen sulfide content: 7 to 8g/Nm3Two stages in series
After three months of operation, the content of the hydrogen sulfide after desulfurization is obviously reduced, and the desulfurization efficiency is improved. The byproducts of ammonium thiosulfate and ammonium sulfate are obviously reduced, and the generation of the byproducts is effectively inhibited.
Second case, removal of hydrogen sulfide from biogas
The using time is 2020, 2 months and 3 months.
The biogas yield is as follows: 5000Nm3H hydrogen sulfide content: 10 to 12g/Nm3(ii) a Single tower operation.
After three months of operation, the content of the hydrogen sulfide after desulfurization is obviously reduced, and the desulfurization efficiency is improved. The byproducts of sodium thiosulfate and sodium sulfate are obviously reduced, the generation of byproduct is effectively inhibited, the sediment is obviously reduced, and favorable conditions are provided for the stable operation of the system.
And in the third use case, the hydrogen sulfide in the sulfur-containing tail gas of a certain pharmaceutical factory is removed. Tail gas yield: 20000Nm3H hydrogen sulfide content: 18 to 20g/Nm3(ii) a The double columns operate in series.
The using time is 2019, 6 months, and the data monitoring time is five months.
After the operation is carried out for five months,
1. the content of hydrogen sulfide after desulfurization is obviously reduced, and the desulfurization efficiency is improved.
2. The byproducts of sodium thiosulfate and sodium sulfate are obviously reduced, and the generation of byproduct is effectively inhibited.
3. The degradation products are obviously reduced, part of substances deposited in the system is brought out in the operation, the system resistance is reduced by about 0.8kpa, and favorable conditions are provided for the stable operation of the system.
Claims (7)
1. A preparation method of a complex iron catalyst for wet desulphurization is characterized by comprising the following steps: the method comprises the following steps: (1) adding phthalic anhydride and fuming sulfuric acid into a reaction kettle, heating to 200-240 ℃ until the reaction is completed, and obtaining sulfophthalic acid; (2) adding sodium hydroxide into sulfophthalic acid, and stirring until the reaction is completed to obtain a compound I; (3) heating the compound I and cobalt chloride to 200-240 ℃ for reaction to obtain a compound II; (4) heating the compound I and an iron-containing compound to 200-240 ℃ for reaction to obtain a compound III; (5) heating the compound II and the compound III to 240-280 ℃ for reaction to obtain a compound IV; (6) preparing a stabilizer: uniformly mixing ATMP, water, ammonia water and citric acid to prepare a bistable agent; (7) and (3) uniformly mixing the compound IV and a bistable agent, heating to 80 ℃, keeping the temperature constant for one hour, cooling and drying to obtain the catalyst.
2. The method for preparing a catalyst according to claim 1, characterized in that: the mass ratio of the phthalic anhydride to the fuming sulfuric acid is 1-2: 1.
3. The method for preparing a catalyst according to claim 1, characterized in that: the mass ratio of ATMP, water, ammonia water and citric acid is 1:1-5:0.05-0.15: 0.05-0.15.
4. The method for preparing a catalyst according to claim 3, characterized in that: the mass ratio of ATMP, water, ammonia water and citric acid is 1:3:0.1: 0.1.
5. The method for preparing a catalyst according to claim 1, characterized in that: the mass ratio of the compound IV to the bistable agent is 2-5: 1.
6. The method for preparing a catalyst according to claim 5, characterized in that: the mass ratio of the compound IV to the bistable agent is 3: 1.
7. The method for preparing a catalyst according to claim 1, characterized in that: the iron-containing compound is ferric hydroxide or ferric chloride.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112316983A (en) * | 2020-10-27 | 2021-02-05 | 宁波中科远东催化工程技术有限公司 | Complex iron desulfurization catalyst and preparation method thereof |
| CN114558622A (en) * | 2022-03-22 | 2022-05-31 | 东南大学 | Desulfurization catalyst for synergistically removing hydrogen sulfide and carbonyl sulfide and preparation method thereof |
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Application publication date: 20200828 |