CN111467937A - High-efficiency desulfurizer and preparation method thereof - Google Patents
High-efficiency desulfurizer and preparation method thereof Download PDFInfo
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- CN111467937A CN111467937A CN202010299915.2A CN202010299915A CN111467937A CN 111467937 A CN111467937 A CN 111467937A CN 202010299915 A CN202010299915 A CN 202010299915A CN 111467937 A CN111467937 A CN 111467937A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
- B01D53/52—Hydrogen sulfide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/10—Inorganic absorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/10—Inorganic absorbents
- B01D2252/102—Ammonia
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/304—Hydrogen sulfide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1456—Removing acid components
- B01D53/1468—Removing hydrogen sulfide
Abstract
The invention relates to the technical field of desulfurization, and particularly discloses a high-efficiency desulfurizing agent and a preparation method thereof. The high-efficiency desulfurizer comprises the following components in parts by weight: 0.4-1 part of ferric nitrate, 2-10 parts of chelating agent, 10-15 parts of hydrogen sulfide absorbent, 2-5 parts of sodium thiosulfate, 1-5 parts of corrosion inhibitor and 1100 parts of water 900-; the chelating agent is iminodisuccinic acid or iminodisuccinate. The high-efficiency desulfurizer provided by the invention has the advantages of no toxicity and harm to an ecological system, no secondary pollution, good stability, simple raw material composition and low desulfurization cost, and can keep higher desulfurization efficiency and higher sulfur capacity under conventional operation.
Description
Technical Field
The invention relates to the technical field of desulfurization, in particular to a high-efficiency desulfurizing agent and a preparation method thereof.
Background
Hydrogen sulfide is a corrosive and irritant acidic harmful gas, and is an industrial waste gas generated along with industrial production. The low concentration of hydrogen sulfide can cause serious harm to the atmospheric environment and human health. The natural gas is widely applied to chemical industry and civil use, and contains impurities such as hydrogen sulfide, the hydrogen sulfide forms weak acid when meeting water, and the existence of the weak acid can cause corrosion of steel equipment and pipelines. Further, when natural gas containing hydrogen sulfide is used as a domestic fuel, sulfide is contained in exhaust gas generated by burning natural gas. Therefore, the natural gas produced by exploitation needs to be subjected to hydrogen sulfide removal firstly so as to meet the use requirements of factory production and civil gas.
In the existing desulfurization process, the complexing iron chelating agent in the desulfurizing agent mainly comprises ethylene diamine tetraacetic acid, diethylenetriamine pentaacetic acid, 1, 2-cyclohexane diamine tetraacetic acid, hydroxyethyl triacetic acid, nitrilotriacetic acid and the like. Although the chelating agent has strong coordination capacity and is easy to form a chelate with heavy metal to increase the solubility of the heavy metal, the chelating agent has the defect of difficult degradation treatment, and the heavy metal is easy to accumulate in water to pollute the water body and has great harm.
Although most of the existing improved desulfurizing agents improve the sulfur capacity, the desulfurizing reaction rate of the desulfurizing agent is slow, the desulfurizing efficiency is low, the sulfur capacity is still not ideal, and the regeneration of the desulfurizing agent after desulfurization consumes a long time. If the wet desulphurization is carried out, a large amount of desulphurization solution is needed for recycling, and the desulphurization solution has the problems of poor stability, multiple side reactions and high sulfur consumption, thereby greatly increasing the desulphurization cost.
Disclosure of Invention
The invention provides a high-efficiency desulfurizer and a preparation method thereof, aiming at the problems that the existing desulfurizer is low in desulfurization efficiency, poor in stability and more in side reactions, and the desulfurizer is long in regeneration time after desulfurization, high in desulfurization cost and difficult to biodegrade to cause environmental pollution.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
the high-efficiency desulfurizer comprises the following components in parts by weight:
0.4-1 part of ferric nitrate, 2-10 parts of chelating agent, 10-15 parts of hydrogen sulfide absorbent, 2-5 parts of sodium thiosulfate, 1-5 parts of corrosion inhibitor and 1100 parts of water 900-;
the chelating agent is iminodisuccinic acid or iminodisuccinate.
Compared with the prior art, the high-efficiency desulfurizer provided by the invention has the advantages of no toxicity, no harm, no secondary pollution to an ecological system, good stability, simple raw material composition and low desulfurization cost, and can keep higher desulfurization efficiency and higher sulfur capacity under conventional operation.
The chelating agent (the iminodisuccinic acid and the iminodisuccinate) has better complexing ability, can effectively prevent ferric nitrate and other components in the desulfurizer from generating precipitation in the solution by adding the chelating agent, and can ensure the solution performance stability of the desulfurizer. The ferric nitrate is a cheap industrial product, can reduce the raw material cost of the desulfurizer, and can be used as a soluble ferric salt which is added into the desulfurizer containing the iminodisuccinic acid or the iminodisuccinic acid salt to obviously increase the desulfurization efficiency and the sulfur capacity of the desulfurizer.
In order to improve the stability of the traditional liquid desulfurizer in the desulfurization process, a complex iron chelating agent with high stability and strong coordination capacity is usually added into the desulfurizer, and although the chelating agent improves the stability of the desulfurizer, the chelating agent is very difficult to degrade in the later period, and heavy metals are easily accumulated in water to cause water body pollution. The ferric nitrate is added into the desulfurizer to be combined with the iminodisuccinic acid or the iminodisuccinate, so that the biodegradation of the chelating agent can be promoted, the biodegradation rate of the chelating agent can reach more than 99 percent under the action of biomass degrading enzyme, the water pollution caused by accumulation of heavy metal in water is avoided, and the desulfurizer is nontoxic and harmless to an ecosystem and is environment-friendly.
According to the desulfurizer, through the matching of the hydrogen sulfide absorbent and the iminodisuccinic acid/iminodisuccinate, the oxidative degradation of the chelating agent in the desulfurization process can be avoided, the stability of the chelating agent in the desulfurizer is improved, the oxidative degradation rate of the chelating agent in the desulfurization operation process is ensured to be lower than 1%, and the stability and higher desulfurization efficiency of the desulfurizer in the operation process are ensured all the time.
Preferably, the composition comprises the following components in parts by weight: 0.6-0.8 part of ferric nitrate, 3-5 parts of chelating agent, 11-13 parts of hydrogen sulfide absorbent, 2-4 parts of sodium thiosulfate, 2-3 parts of corrosion inhibitor and 1050 parts of water 950-.
Preferably, the composition comprises the following components in parts by weight: 0.7 part of ferric nitrate, 4 parts of chelating agent, 12 parts of hydrogen sulfide absorbent, 3 parts of sodium thiosulfate, 2.5 parts of corrosion inhibitor and 1000 parts of water.
The above-mentioned preferable component ratio can further improve the desulfurization rate and the stability of the desulfurizing agent.
Preferably, the iminodisuccinate salt is one of iminodisuccinate sodium salt, iminodisuccinate potassium salt, iminodisuccinate iron salt and iminodisuccinate ammonium salt.
Preferably, the hydrogen sulfide absorbent is sodium carbonate or ammonia water.
Preferably, the corrosion inhibitor is sodium molybdate.
Sodium molybdate is preferably used as a corrosion inhibitor, so that the desulfurization equipment can be effectively prevented from being corroded by a desulfurizing agent.
The invention also provides a preparation method of the high-efficiency desulfurizing agent. The preparation method comprises the following steps: adding ferric nitrate into water according to the weight ratio, stirring and dissolving, then sequentially adding a chelating agent, sodium thiosulfate, a corrosion inhibitor and a hydrogen sulfide absorbent, dissolving, and then adjusting the pH value to 8-9 to obtain the desulfurizer.
Compared with the prior art, the preparation method of the high-efficiency desulfurizer provided by the invention is simple to operate, low in equipment requirement and low in cost and raw materials are easily available, and compared with the traditional preparation method of the desulfurizer, the raw material cost and the labor cost are both obviously reduced.
Preferably, the pH adjustment is performed with sodium carbonate or ammonia.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The high-efficiency desulfurizer comprises the following components in parts by weight:
0.4 part of ferric nitrate, 2 parts of iminodisuccinic acid sodium salt, 10 parts of sodium carbonate, 2 parts of sodium thiosulfate, 1 part of sodium molybdate and 900 parts of water.
The preparation method of the high-efficiency desulfurizer comprises the following steps:
adding ferric nitrate into water according to the weight ratio, stirring and dissolving, then adding iminodisuccinic acid sodium salt until the iminodisuccinic acid sodium salt is completely dissolved, adding sodium thiosulfate and sodium molybdate to dissolve, then adding sodium carbonate, and adjusting the pH value to 8 to obtain the desulfurizer.
Example 2
The high-efficiency desulfurizer comprises the following components in parts by weight:
0.7 part of ferric nitrate, 4 parts of iminodisuccinic acid sodium salt, 12 parts of ammonia water, 3 parts of sodium thiosulfate, 2.5 parts of sodium molybdate and 1000 parts of water.
The preparation method of the high-efficiency desulfurizer comprises the following steps:
adding ferric nitrate into water according to the weight ratio, stirring and dissolving, then adding iminodisuccinic acid sodium salt until the iminodisuccinic acid sodium salt is completely dissolved, adding sodium thiosulfate and sodium molybdate for dissolving, then adding ammonia water, and adjusting the pH value to 9 to obtain the desulfurizer.
Example 3
The high-efficiency desulfurizer comprises the following components in parts by weight:
1 part of ferric nitrate, 10 parts of imino disuccinic acid ammonium salt, 15 parts of sodium carbonate, 5 parts of sodium thiosulfate, 5 parts of sodium molybdate and 1100 parts of water.
The preparation method of the high-efficiency desulfurizer comprises the following steps:
adding ferric nitrate into water according to the weight ratio, stirring and dissolving, then adding iminodisuccinic acid ammonium salt until the ammonium salt is completely dissolved, adding sodium thiosulfate and sodium molybdate to dissolve, then adding sodium carbonate, and adjusting the pH value to 8 to obtain the desulfurizer.
Example 4
The high-efficiency desulfurizer comprises the following components in parts by weight:
0.6 part of ferric nitrate, 3 parts of iminodisuccinic acid, 11 parts of sodium carbonate, 2 parts of sodium thiosulfate, 2 parts of sodium molybdate and 950 parts of water.
The preparation method of the high-efficiency desulfurizer comprises the following steps:
adding ferric nitrate into water according to the weight ratio, stirring and dissolving, then adding iminodisuccinic acid to completely dissolve, then adding sodium thiosulfate and sodium molybdate to dissolve, then adding sodium carbonate, and adjusting the pH value to 8 to obtain the desulfurizer.
Example 5
The high-efficiency desulfurizer comprises the following components in parts by weight:
0.7 part of ferric nitrate, 4 parts of imino disuccinic acid ferric salt, 12 parts of ammonia water, 3 parts of sodium thiosulfate, 2.5 parts of sodium molybdate and 1000 parts of water.
The preparation method of the high-efficiency desulfurizer comprises the following steps:
adding ferric nitrate into water according to the weight ratio, stirring and dissolving, then adding imino disuccinic acid ferric salt, adding sodium thiosulfate and sodium molybdate to dissolve after completely dissolving, adding ammonia water, and adjusting the pH value to 9 to obtain the desulfurizer.
Example 6
The high-efficiency desulfurizer comprises the following components in parts by weight:
0.8 part of ferric nitrate, 5 parts of iminodisuccinic acid potassium salt, 13 parts of sodium carbonate, 4 parts of sodium thiosulfate, 3 parts of sodium molybdate and 1050 parts of water.
The preparation method of the high-efficiency desulfurizer comprises the following steps:
adding ferric nitrate into water according to the weight ratio, stirring and dissolving, then adding potassium iminodisuccinate until the potassium iminodisuccinate is completely dissolved, adding sodium thiosulfate and sodium molybdate to dissolve, then adding sodium carbonate, and adjusting the pH value to 8 to obtain the desulfurizer.
Comparative example 1
The same amount of sodium sulfosalicylate as that of the iminodisuccinate in example 1 was used instead of the sodium iminodisuccinate in example 1, and the other components and the preparation method were the same as in example 1, to obtain a desulfurizing agent.
Comparative example 2
The same amount of iron sulfate was used instead of the iron nitrate in example 1, and the other components and preparation method were the same as in example 1, to obtain a desulfurizing agent.
Comparative example 3
The same amount of sodium benzenesulfonate as that used in example 1 was used instead of sodium thiosulfate in example 1, and the other components and preparation method were the same as those in example 1, to obtain a desulfurizing agent.
The desulfurizing agents obtained in the examples 1 to 6 and the comparative examples 1 to 3 are placed in a desulfurizing device, and the coke oven gas is desulfurized under the following processing conditions:
the flow rate of coke oven gas is 100L/h;
the flow rate of the desulfurizer is 2L/h;
the air aeration flow rate is 40L/h;
temperature: at 20 ℃.
And after 72h of desulfurization treatment, detecting the desulfurization effect and the sulfur capacity of the desulfurizer, wherein the detection results are shown in table 1:
TABLE 1 desulfurization efficiency and sulfur capacity
The desulfurization efficiency of the desulfurizing agent obtained in the embodiments 1-6 is above 99.6% after the desulfurizing agent runs for 72 hours in a desulfurizing device, which shows that the desulfurizing agent has high desulfurization efficiency, can ensure that the coke oven gas reaches the purification standard, does not generate precipitates in the desulfurizing agent after the desulfurizing agent runs for 72 hours, has excellent stability, and has the highest sulfur capacity of 2.41 g/L and good service performance.
The degradation rate of the chelating agent in the desulfurizing agent is detected, and the detection result is shown in table 2:
TABLE 2 oxidative degradation rate of chelating agent
Wherein, the oxidative degradation rate of the chelating agent is (the concentration of the chelating agent in the initial desulfurizing agent-the concentration of the chelating agent in the desulfurizing agent after 72 h)/the concentration of the chelating agent in the initial desulfurizing agent.
The desulfurizing agents in examples 1 to 6 run in the desulfurizing device for 72 hours, and the degradation rate of the chelating agent in the desulfurizing agent is low, which shows that the chelating agent in the desulfurizing agent has low oxidative degradation rate and good stability in the using process.
The iron consumption rate in the desulfurizing agent was measured, and the measurement results are shown in table 3:
TABLE 3 iron consumption Rate
The iron consumption rate is (the total iron concentration in the initial desulfurizer is-72 h), and the total iron concentration in the initial desulfurizer is calculated.
The desulfurizing agents of examples 1 to 6 were operated in the desulfurizing device for 72 hours, and the iron consumption rate in the desulfurizing agent was low, indicating that the desulfurizing agent of the present invention has a strong complexing ability to iron.
The biodegradation efficiency of the chelating agent in the desulfurizer is detected, and the detection method comprises the following steps: 0.5 wt% of biomass degrading enzyme is added into the desulfurizer, the mixture is treated for 24 hours at 35 ℃, and the detection results are shown in Table 4:
TABLE 4 biodegradation efficiency of chelating Agents
The biodegradation rate of the chelating agent is ═ (concentration of the chelating agent in the initial desulfurizing agent-concentration of the chelating agent in the desulfurizing agent after the treatment with the biomass degrading enzyme)/concentration of the chelating agent in the initial desulfurizing agent.
After the desulfurizer in the embodiments 1 to 6 is treated by the biomass degrading enzyme, the degradation rate of the chelating agent in the desulfurizer reaches more than 99 percent, which shows that the chelating agent in the desulfurizer of the invention has good biodegradation rate and does not cause secondary pollution to the environment.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (8)
1. A high-efficiency desulfurizer is characterized in that: the paint comprises the following components in parts by weight:
0.4-1 part of ferric nitrate, 2-10 parts of chelating agent, 10-15 parts of hydrogen sulfide absorbent, 2-5 parts of sodium thiosulfate, 1-5 parts of corrosion inhibitor and 1100 parts of water 900-;
the chelating agent is iminodisuccinic acid or iminodisuccinate.
2. The efficient desulfurizing agent according to claim 1, wherein: the paint comprises the following components in parts by weight: 0.6-0.8 part of ferric nitrate, 3-5 parts of chelating agent, 11-13 parts of hydrogen sulfide absorbent, 2-4 parts of sodium thiosulfate, 2-3 parts of corrosion inhibitor and 1050 parts of water 950-.
3. The efficient desulfurizing agent according to claim 1, wherein: the paint comprises the following components in parts by weight: 0.7 part of ferric nitrate, 4 parts of chelating agent, 12 parts of hydrogen sulfide absorbent, 3 parts of sodium thiosulfate, 2.5 parts of corrosion inhibitor and 1000 parts of water.
4. The high efficiency desulfurizing agent according to any one of claims 1 to 3, wherein: the iminodisuccinate is one of iminodisuccinate sodium salt, iminodisuccinate potassium salt, iminodisuccinate iron salt and iminodisuccinate ammonium salt.
5. The high efficiency desulfurizing agent according to any one of claims 1 to 3, wherein: the hydrogen sulfide absorbent is sodium carbonate or ammonia water.
6. The high efficiency desulfurizing agent according to any one of claims 1 to 3, wherein: the corrosion inhibitor is sodium molybdate.
7. The method for preparing the high-efficiency desulfurizing agent according to any one of claims 1 to 6, wherein the desulfurizing agent comprises: adding ferric nitrate into water according to the weight ratio, stirring and dissolving, then sequentially adding a chelating agent, sodium thiosulfate, a corrosion inhibitor and a hydrogen sulfide absorbent, dissolving, and then adjusting the pH value to 8-9 to obtain the desulfurizer.
8. The method for preparing the high efficiency desulfurizing agent according to claim 7, wherein: adjusting pH value with sodium carbonate or ammonia water.
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CN112058044A (en) * | 2020-09-07 | 2020-12-11 | 四川沃兹凯兰科技有限公司 | Selective wet desulfurizing agent and preparation method thereof |
CN112973404A (en) * | 2021-03-17 | 2021-06-18 | 河北络合科技有限公司 | Complex iron desulfurizer and preparation method and application thereof |
CN113215413A (en) * | 2021-04-13 | 2021-08-06 | 华南理工大学 | Desulfurizing agent and method for preparing zero-carbon smelting precursor by removing sulfur in waste lead paste |
CN114632408A (en) * | 2022-04-11 | 2022-06-17 | 湖南煤化新能源有限公司 | Dry quenching flue gas treatment system and method thereof |
CN115845924A (en) * | 2022-12-22 | 2023-03-28 | 河北络合科技有限公司 | Catalyst for biogas desulfurization and preparation method and application thereof |
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Cited By (6)
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CN112058044A (en) * | 2020-09-07 | 2020-12-11 | 四川沃兹凯兰科技有限公司 | Selective wet desulfurizing agent and preparation method thereof |
CN112973404A (en) * | 2021-03-17 | 2021-06-18 | 河北络合科技有限公司 | Complex iron desulfurizer and preparation method and application thereof |
CN113215413A (en) * | 2021-04-13 | 2021-08-06 | 华南理工大学 | Desulfurizing agent and method for preparing zero-carbon smelting precursor by removing sulfur in waste lead paste |
CN114632408A (en) * | 2022-04-11 | 2022-06-17 | 湖南煤化新能源有限公司 | Dry quenching flue gas treatment system and method thereof |
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CN115845924A (en) * | 2022-12-22 | 2023-03-28 | 河北络合科技有限公司 | Catalyst for biogas desulfurization and preparation method and application thereof |
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