Desulfurizing agent for oil extraction in oil-gas field and preparation method thereof

By combining N-octadecyl-1,3-propanediamine, ionic liquid@organic copper mixture, ammonium molybdate and other components to form a desulfurizing agent, the problem of poor removal efficiency of inorganic and organic sulfur in existing technologies has been solved, achieving efficient and stable hydrogen sulfide treatment and reducing the dosage and equipment corrosion risk.

CN121319974AActive Publication Date: 2026-01-13SHENGLI OILFIELD HAIFA ENVIRONMENTAL PROTECTION CHEM CO LTD +1
View PDF 9 Cites 0 Cited by

Patent Information

Application Number
CN202511906674.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-17
Publication Date
2026-01-13
Estimated Expiration
2045-12-17

AI Technical Summary

Technical Problem

Existing desulfurizing agents used in oil and gas field production are not effective at removing inorganic and organic sulfur, and require large quantities and have poor compatibility, making it difficult to effectively treat harmful gases such as hydrogen sulfide and mercaptans.

Method used

A desulfurizing agent composed of N-octadecyl-1,3-propanediamine, ionic liquid@organic copper mixture, ammonium molybdate, sodium lysine, hydroxyethylidene diphosphonic acid, and polyoxyethylene sorbitan monostearate achieves efficient removal of inorganic and organic sulfur through synergistic effects. It utilizes the hydrophilic and lipophilic properties of the ionic liquid, the catalytic effect of copper naphthenate, and the interfacial adsorption of N-octadecyl-1,3-propanediamine to form stable chelates and chemical neutralization reactions.

Benefits of technology

It achieves efficient removal of inorganic and organic sulfur, reduces the risk of equipment corrosion, improves the stability and permeability of the desulfurizing agent, enhances the treatment effect of hydrogen sulfide, and reduces the amount used.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure SMS_1
    Figure SMS_1
  • Figure SMS_2
    Figure SMS_2
Patent Text Reader

Abstract

The invention belongs to the technical field of desulfurizer preparation, and particularly relates to a desulfurizer for oil extraction of oil and gas fields and a preparation method thereof. The desulfurizing agent for oil extraction of the oil and gas field is prepared from the following raw materials: N-octadecyl-1, 3-propane diamine, an ionic liquid and organic copper mixture, ammonium molybdate, lysine sodium, hydroxyethylidene diphosphonic acid, polyoxyethylene sorbitan monostearate and the balance of water. According to the desulfurizing agent for oil extraction of the oil-gas field, water is used as a solvent, N-octadecyl-1, 3-propane diamine, an ionic liquid and organic copper mixture and ammonium molybdate in raw materials are used as main desulfurizing components to remove organic sulfur and inorganic sulfur, and lysine sodium, hydroxyethylidene diphosphonic acid and polyoxyethylene sorbitan monostearate are added, so that the desulfurizing agent for oil extraction of the oil-gas field is obtained. Due to the synergistic effect of the raw materials, the efficient removal of inorganic sulfur and organic sulfur in oil extraction of an oil and gas field is realized.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention belongs to the field of desulfurization agent preparation technology, specifically relating to a desulfurization agent for oil and gas field production and its preparation method. Background Technology

[0002] Hydrogen sulfide, a highly toxic gas, is often generated during oil and gas field development, posing a significant hazard to both personnel and equipment. Effective prevention and control of hydrogen sulfide is crucial for the safe development of oil and gas fields. To ensure personal safety, prevent hydrogen sulfide poisoning incidents, reduce the harm of hydrogen sulfide to production equipment, and minimize its environmental pollution, it is essential to strengthen preventative and control measures for hydrogen sulfide. The mechanism of hydrogen sulfide generation mainly includes the following three aspects: (1) Deep within oil and gas reservoirs, there are usually large amounts of sulfate-reducing bacteria. Formation temperature and the abundance of ammonium and nitrate ions in the formation provide favorable conditions for their growth. The metabolic products of sulfate-reducing bacteria contain large amounts of hydrogen sulfide. Furthermore, during oil and gas field development, water injection wells inject water into the oil layer to protect its pressure; some untreated wastewater often contains sulfate-reducing bacteria. (2) Hydrogen sulfide is often generated in the metabolic and degradation products of organisms. (III) The thermochemical reduction of sulfates causes natural gas to generate high abundance of hydrogen sulfide. During the extraction of oil and gas fields, crude oil contains a certain amount of organic sulfides such as hydrogen sulfide, methanethiol, ethanethiol, and carbonyl sulfide.

[0003] Patent CN111944560A discloses a desulfurizing agent for oil and gas fields, comprising a liquid triazine-based desulfurizing agent, and adding a scaling inhibitor, a synergist, and a dispersant. The liquid triazine-based desulfurizing agent has a mass fraction of 60-80%, the scaling inhibitor has a mass fraction of 5-10%, the synergist has a mass fraction of 5-10%, and the dispersant has a mass fraction of the remainder. While the triazine-based desulfurizing agent in the above patent can effectively remove hydrogen sulfide, its effect on other sulfur-containing odorous gases such as mercaptans is very limited.

[0004] Currently, desulfurizing agents used in oil and gas field production suffer from various problems, including low desulfurization efficiency (effective at removing inorganic sulfur but poor at removing organic sulfur such as thiols and carbonyl sulfur), large dosage, and poor compatibility. Therefore, it is necessary to explore a new type of desulfurizing agent for oil and gas field production. Summary of the Invention

[0005] The purpose of this invention is to provide a desulfurizing agent for oil and gas field production, which has a good removal effect on both inorganic and organic sulfur. In addition, this invention also provides a method for its preparation.

[0006] The desulfurizing agent for oil and gas field production of the present invention is composed of the following raw materials by mass percentage: 3.5-3.7% N-octadecyl-1,3-propanediamine, 13-15% ionic liquid@organic copper mixture, 4.0-4.5% ammonium molybdate, 2.7-3.3% sodium lysine, 0.8-1.0% hydroxyethylidene diphosphonic acid, 1.0-1.5% polyoxyethylene sorbitan monostearate, and water as the balance; wherein, the preparation method of the ionic liquid@organic copper mixture is as follows: firstly, 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is vacuum dried, and after the vacuum is stopped, copper naphthenate is added to it under nitrogen protection and stirred at room temperature. After cooling to room temperature, the ionic liquid@organic copper mixture is obtained.

[0007] In the preparation method of the ionic liquid@organic copper mixture, the vacuum drying temperature is 80℃, the vacuum drying pressure is -0.09MPa, and the vacuum drying time is 55-60min.

[0008] In the preparation method of ionic liquid@organic copper mixture, the stirring speed is 100 r / min and the stirring time is 15 min.

[0009] In the preparation method of ionic liquid@organic copper mixture, the mass ratio of copper naphthenate to 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is 1:1.5.

[0010] The method for preparing the desulfurizing agent for oil and gas field production according to the present invention comprises the following steps: (1) Add the ionic liquid@organic copper mixture to the reaction apparatus, heat to 40-42℃ and stir to dissolve it; (2) Add N-octadecyl-1,3-propanediamine, heat to 50-52℃ and continue stirring until the solution is homogeneous; (3) Add hydroxyethylidene diphosphonic acid and stir until completely dispersed; (4) Add ammonium molybdate to the reaction system of step (3) in three portions, with an interval of 5 minutes between each addition, and stir to mix thoroughly. (5) Add sodium lysine and stir until well mixed. Then add polyoxyethylene sorbitan monostearate, heat to 54-56℃ and continue stirring until uniform. Finally, add deionized water and stir until uniform. After vacuum degassing, the desulfurizing agent for oil and gas field production is prepared.

[0011] Wherein: the stirring speed in step (1) is 100 r / min and the stirring time is 10-15 min.

[0012] The stirring speed in step (2) is 100 r / min, and the stirring time is 10-15 min.

[0013] In step (2), when the system is heated to 50-52℃, the heating rate is controlled at 1℃ / min during the heating process to prevent local overheating that could lead to copper oxidation or amine precipitation.

[0014] The stirring speed in step (3) is 150 r / min, and the stirring time is 5-7 min.

[0015] In step (4), the mass of ammonium molybdate added each time is equal, and after the three additions are completed, continue stirring for 15 minutes.

[0016] The stirring speed in step (4) is 150 r / min.

[0017] In step (5), add sodium lysine and stir for 5-7 minutes at a stirring speed of 200 r / min. Add polyoxyethylene sorbitan monostearate and stir for 10-13 minutes at a stirring speed of 200 r / min. Finally, add deionized water and stir for 12-15 minutes at a stirring speed of 200 r / min. The vacuum degassing pressure is -0.09 MPa, the vacuum degassing time is 10 minutes, and the stirring speed during vacuum degassing is 50 r / min.

[0018] In step (5), when the system is heated to 54-56℃, the heating rate is controlled at 1℃ / min during the heating process to prevent local overheating that could lead to copper oxidation or amine precipitation.

[0019] When adding deionized water in step (5), first preheat the deionized water to 43-45℃ and then add it at a constant rate to avoid instantaneous cooling that could cause the emulsion phase to separate.

[0020] Compared with the prior art, the present invention has the following advantages: (1) The desulfurizing agent for oil and gas field production described in this invention uses water as a solvent. The N-octadecyl-1,3-propanediamine, ionic liquid@organic copper mixture and ammonium molybdate in the raw materials are used as the main desulfurizing components to remove organic sulfur and inorganic sulfur. Sodium lysine, hydroxyethylidene diphosphonic acid and polyoxyethylene sorbitan monostearate are added to enhance the stability and permeability of the system. Thus, the raw materials work synergistically to achieve efficient removal of inorganic sulfur and organic sulfur in oil and gas field production.

[0021] (2) The desulfurizing agent for oil and gas field production described in this invention uses N-octadecyl-1,3-propanediamine, an ionic liquid@organic copper mixture, and ammonium molybdate as the main desulfurizing components. The three components work synergistically to remove inorganic and organic sulfur. Among them, the sulfonic acid group and imidazole ring of 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate in the ionic liquid@organic copper mixture have hydrophilic and lipophilic properties, which can reduce the interfacial tension between oil and water, making it easier for thiols to accumulate at the oil-water interface. Copper naphthenate slowly releases Cu in the oil phase. 2+ Cu2+ It forms a stable coordination chelate (Cu-SR) with the sulfur atom in thiols, which is then separated during subsequent processing in crude oil gathering and transportation. For carbonyl sulfides: the sulfonic acid group of the ionic liquid has an acidic site that can catalyze the hydrolysis of carbonyl sulfides, producing hydrogen sulfide and carbon dioxide. The H2S generated during hydrolysis immediately reacts with the released Cu... 2+ The reaction produces copper sulfide precipitate or stable Cu-SH complex, preventing secondary release of H2S; however, for inorganic sulfur: copper naphthenate in the mixture can completely dissolve in the oil phase, releasing Cu at the oil-water interface. 2+ Upon contact with hydrogen sulfide, it forms copper sulfide grains, which are carried away by the oil flow, reducing the risk of clogging rock pores and throats. N-Octadecyl-1,3-propanediamine utilizes C... 18 The long-chain lipophilic and diamine hydrophilic structure allows for directional adsorption at the oil-water interface, forming a monolayer that reduces interfacial tension and facilitates wetting of the rock and crude oil by subsequent aqueous desulfurizing agents. The amine group in the N-octadecyl-1,3-propanediamine molecule exhibits strong basicity, enabling it to chemically neutralize inorganic sulfur (H₂S) to form an amine salt, thus removing the inorganic sulfur. The molybdenum in ammonium molybdate forms a "Cu-Mo dual active center" with the copper in the ionic liquid@organic copper mixture, exhibiting excellent catalytic activity in breaking the chemical bonds of difficult-to-remove organic sulfur, thereby improving the removal rate of stubborn sulfur.

[0022] (3) The desulfurizing agent for oil and gas field production described in this invention also contains sodium lysine, polyoxyethylene sorbitan monostearate, and hydroxyethylidene diphosphonic acid in its raw materials. Specifically, the sodium carboxylate group (hydrophilic) and alkyl chain (lipophilic) in the sodium lysine molecule work synergistically to reduce the viscosity of the main system and assist in the dispersion of ammonium molybdate and Cu. 2+ The active ingredients prevent aggregation, improve compatibility with crude oil, increase the contact area for desulfurization reactions, and possess good salt resistance. Their dispersing effect alleviates system aggregation caused by high salt content. Polyoxyethylene sorbitan monostearate, as a nonionic surfactant, first reduces the oil-water interfacial tension, making it easier for the aqueous phase to spread on the rock and oil film surfaces, thereby allowing the desulfurizer to penetrate deeper into the oil phase and improve sulfur capture efficiency. Hydroxyethylidene diphosphonic acid and Cu... 2+ Mo 6+ It forms weakly coordinated chelates, inhibiting hydrolysis and precipitation under high temperature and high salt conditions, and prolonging the activity cycle of the desulfurizer. When there are no sulfides in the system, the weak coordination of hydroxyethylidene diphosphonic acid will "temporarily store" metal ions, preventing them from hydrolyzing and precipitating. When sulfides such as thiols, carbonyl sulfides, and thiophenes are present in the system, the metal ions will preferentially combine with the sulfides and be "released" from the coordination of hydroxyethylidene diphosphonic acid to participate in the desulfurization reaction. It has a good catalytic effect on the breaking of the chemical bond of sulfur and can improve the removal rate of stubborn sulfur.

[0023] (4) The preparation method of the desulfurizing agent for oil and gas field production described in this invention is simple, the parameters are easy to control, and the prepared desulfurizing agent for oil and gas field production has stable performance. Detailed Implementation

[0024] Example 1 The desulfurizing agent for oil and gas field production described in Example 1 is composed of the following raw materials by mass percentage: 3.6% N-octadecyl-1,3-propanediamine, 14% ionic liquid@organic copper mixture, 4.3% ammonium molybdate, 2.9% sodium lysine, 0.9% hydroxyethylidene diphosphonic acid, 1.3% polyoxyethylene sorbitan monostearate, and water as the balance. The preparation method of the ionic liquid@organic copper mixture is as follows: first, 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is dried under vacuum. After the vacuum is stopped, copper naphthenate is added to it under nitrogen protection and stirred at room temperature. The mixture is then cooled to room temperature to obtain the ionic liquid@organic copper mixture.

[0025] In the preparation method of the ionic liquid@organic copper mixture, the vacuum drying temperature is 80℃, the vacuum drying pressure is -0.09MPa, and the vacuum drying time is 58min.

[0026] In the preparation method of ionic liquid@organic copper mixture, the stirring speed is 100 r / min and the stirring time is 15 min.

[0027] In the preparation method of ionic liquid@organic copper mixture, the mass ratio of copper naphthenate to 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is 1:1.5.

[0028] The preparation method of the desulfurizing agent for oil and gas field production described in Example 1 consists of the following steps: (1) Add the ionic liquid@organic copper mixture to the reaction apparatus, heat to 41°C and stir to dissolve it; (2) Add N-octadecyl-1,3-propanediamine, heat to 51°C and continue stirring until the solution is homogeneous; (3) Add hydroxyethylidene diphosphonic acid and stir until completely dispersed; (4) Add ammonium molybdate to the reaction system of step (3) in three portions, with an interval of 5 minutes between each addition, and stir to mix thoroughly. (5) Add sodium lysine and stir until well mixed. Then add polyoxyethylene sorbitan monostearate, heat to 55°C and continue stirring until uniform. Finally, add deionized water and stir until uniform. After vacuum degassing, the desulfurizing agent for oil and gas field production is prepared.

[0029] Wherein: the stirring speed in step (1) is 100 r / min and the stirring time is 13 min.

[0030] In step (2), the stirring speed is 100 r / min and the stirring time is 13 min.

[0031] In step (2), when the system is heated to 51°C, the heating rate is controlled at 1°C / min during the heating process to prevent local overheating that could lead to copper oxidation or amine precipitation.

[0032] The stirring speed in step (3) is 150 r / min and the stirring time is 6 min.

[0033] In step (4), the mass of ammonium molybdate added each time is equal, and after the three additions are completed, continue stirring for 15 minutes.

[0034] The stirring speed in step (4) is 150 r / min.

[0035] In step (5), sodium lysine is added and stirred for 6 minutes at a stirring speed of 200 r / min. Polyoxyethylene sorbitan monostearate is added and stirred for 11 minutes at a stirring speed of 200 r / min. Finally, deionized water is added and stirred for 13 minutes at a stirring speed of 200 r / min. The vacuum degassing pressure is -0.09 MPa, the vacuum degassing time is 10 minutes, and the stirring speed during vacuum degassing is 50 r / min.

[0036] In step (5), when the system is heated to 55°C, the heating rate is controlled at 1°C / min during the heating process to prevent local overheating that could lead to copper oxidation or amine precipitation.

[0037] When adding deionized water in step (5), the deionized water should first be preheated to 44°C and then added at a constant rate to avoid instantaneous cooling that could cause emulsion phase separation.

[0038] Example 2 The desulfurizing agent for oil and gas field production described in Example 2 is composed of the following raw materials by mass percentage: 3.5% N-octadecyl-1,3-propanediamine, 13% ionic liquid@organic copper mixture, 4.5% ammonium molybdate, 2.7% sodium lysine, 1.0% hydroxyethylidene diphosphonic acid, 1.0% polyoxyethylene sorbitan monostearate, and water as the balance. The preparation method of the ionic liquid@organic copper mixture is as follows: first, 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is dried under vacuum. After the vacuum is stopped, copper naphthenate is added to it under nitrogen protection and stirred at room temperature. The mixture is then cooled to room temperature to obtain the ionic liquid@organic copper mixture.

[0039] In the preparation method of the ionic liquid@organic copper mixture, the vacuum drying temperature is 80℃, the vacuum drying pressure is -0.09MPa, and the vacuum drying time is 55min.

[0040] In the preparation method of ionic liquid@organic copper mixture, the stirring speed is 100 r / min and the stirring time is 15 min.

[0041] In the preparation method of ionic liquid@organic copper mixture, the mass ratio of copper naphthenate to 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is 1:1.5.

[0042] The preparation method of the desulfurizing agent for oil and gas field production described in Example 2 consists of the following steps: (1) Add the ionic liquid@organic copper mixture to the reaction apparatus, heat to 40°C and stir to dissolve it; (2) Add N-octadecyl-1,3-propanediamine, heat to 50°C and continue stirring until the solution is homogeneous; (3) Add hydroxyethylidene diphosphonic acid and stir until completely dispersed; (4) Add ammonium molybdate to the reaction system of step (3) in three portions, with an interval of 5 minutes between each addition, and stir to mix thoroughly. (5) Add sodium lysine and stir until well mixed. Then add polyoxyethylene sorbitan monostearate, heat to 54°C and continue stirring until uniform. Finally, add deionized water and stir until uniform. After vacuum degassing, the desulfurizing agent for oil and gas field production is prepared.

[0043] Wherein: the stirring speed in step (1) is 100 r / min and the stirring time is 10 min.

[0044] The stirring speed in step (2) is 100 r / min and the stirring time is 10 min.

[0045] In step (2), when the system is heated to 50°C, the heating rate is controlled at 1°C / min during the heating process to prevent local overheating that could lead to copper oxidation or amine precipitation.

[0046] The stirring speed in step (3) is 150 r / min and the stirring time is 7 min.

[0047] In step (4), the mass of ammonium molybdate added each time is equal, and after the three additions are completed, continue stirring for 15 minutes.

[0048] The stirring speed in step (4) is 150 r / min.

[0049] In step (5), sodium lysine is added and stirred for 5 minutes at a stirring speed of 200 r / min. Polyoxyethylene sorbitan monostearate is added and stirred for 10 minutes at a stirring speed of 200 r / min. Finally, deionized water is added and stirred for 15 minutes at a stirring speed of 200 r / min. The vacuum degassing pressure is -0.09 MPa, the vacuum degassing time is 10 minutes, and the stirring speed during vacuum degassing is 50 r / min.

[0050] In step (5), when the system is heated to 54°C, the heating rate is controlled at 1°C / min during the heating process to prevent local overheating that could lead to copper oxidation or amine precipitation.

[0051] When adding deionized water in step (5), the deionized water should first be preheated to 43°C and then added at a constant rate to avoid instantaneous cooling that could cause the emulsion phase to separate.

[0052] Example 3 The desulfurizing agent for oil and gas field production described in Example 3 is composed of the following raw materials by mass percentage: 3.7% N-octadecyl-1,3-propanediamine, 15% ionic liquid@organic copper mixture, 4.0% ammonium molybdate, 3.3% sodium lysine, 0.8% hydroxyethylidene diphosphonic acid, 1.5% polyoxyethylene sorbitan monostearate, and water as the balance. The preparation method of the ionic liquid@organic copper mixture is as follows: first, 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is dried under vacuum. After the vacuum is stopped, copper naphthenate is added to it under nitrogen protection and stirred at room temperature. The mixture is then cooled to room temperature to obtain the ionic liquid@organic copper mixture.

[0053] In the preparation method of the ionic liquid@organic copper mixture, the vacuum drying temperature is 80℃, the vacuum drying pressure is -0.09MPa, and the vacuum drying time is 60min.

[0054] In the preparation method of ionic liquid@organic copper mixture, the stirring speed is 100 r / min and the stirring time is 15 min.

[0055] In the preparation method of ionic liquid@organic copper mixture, the mass ratio of copper naphthenate to 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is 1:1.5.

[0056] The preparation method of the desulfurizing agent for oil and gas field production described in Example 3 consists of the following steps: (1) Add the ionic liquid@organic copper mixture to the reaction apparatus, heat to 42°C and stir to dissolve it; (2) Add N-octadecyl-1,3-propanediamine, heat to 52°C and continue stirring until the solution is homogeneous; (3) Add hydroxyethylidene diphosphonic acid and stir until completely dispersed; (4) Add ammonium molybdate to the reaction system of step (3) in three portions, with an interval of 5 minutes between each addition, and stir to mix thoroughly. (5) Add sodium lysine and stir until well mixed. Then add polyoxyethylene sorbitan monostearate, heat to 56°C and continue stirring until uniform. Finally, add deionized water and stir until uniform. After vacuum degassing, the desulfurizing agent for oil and gas field production is prepared.

[0057] Wherein: the stirring speed in step (1) is 100 r / min and the stirring time is 15 min.

[0058] The stirring speed in step (2) is 100 r / min and the stirring time is 15 min.

[0059] In step (2), when the system is heated to 52°C, the heating rate is controlled at 1°C / min during the heating process to prevent local overheating that could lead to copper oxidation or amine precipitation.

[0060] The stirring speed in step (3) is 150 r / min and the stirring time is 5 min.

[0061] In step (4), the mass of ammonium molybdate added each time is equal, and after the three additions are completed, continue stirring for 15 minutes.

[0062] The stirring speed in step (4) is 150 r / min.

[0063] In step (5), sodium lysine is added and stirred for 7 minutes at a stirring speed of 200 r / min. Polyoxyethylene sorbitan monostearate is added and stirred for 13 minutes at a stirring speed of 200 r / min. Finally, deionized water is added and stirred for 12 minutes at a stirring speed of 200 r / min. The vacuum degassing pressure is -0.09 MPa, the vacuum degassing time is 10 minutes, and the stirring speed during vacuum degassing is 50 r / min.

[0064] In step (5), when the system is heated to 56°C, the heating rate is controlled at 1°C / min during the heating process to prevent local overheating that could lead to copper oxidation or amine precipitation.

[0065] When adding deionized water in step (5), the deionized water should first be preheated to 45°C and then added at a constant rate to avoid instantaneous cooling that could cause emulsion phase separation.

[0066] Comparative Example 1 The preparation method of the desulfurizing agent for oil and gas field production described in Comparative Example 1 is the same as that in Example 1, except that the raw material composition is different. The desulfurizing agent for oil and gas field production described in Comparative Example 1 is composed of the following raw materials by mass percentage: 14% ionic liquid@organic copper mixture, 4.3% ammonium molybdate, 2.9% sodium lysine, 0.9% hydroxyethylidene diphosphonic acid, 1.3% polyoxyethylene sorbitan monostearate, and water as the balance; wherein, the preparation method of the ionic liquid@organic copper mixture is as follows: first, 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is dried under vacuum, and after the vacuum is stopped, copper naphthenate is added to it under nitrogen protection and stirred at room temperature. After cooling to room temperature, the ionic liquid@organic copper mixture is obtained.

[0067] In the preparation method of the ionic liquid@organic copper mixture, the vacuum drying temperature is 80℃, the vacuum drying pressure is -0.09MPa, and the vacuum drying time is 58min.

[0068] In the preparation method of ionic liquid@organic copper mixture, the stirring speed is 100 r / min and the stirring time is 15 min.

[0069] In the preparation method of ionic liquid@organic copper mixture, the mass ratio of copper naphthenate to 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is 1:1.5.

[0070] Comparative Example 2 The preparation method of the desulfurizing agent for oil and gas field production described in Comparative Example 2 is the same as that in Example 1, the only difference being the composition of the raw materials. The desulfurizing agent for oil and gas field production described in Comparative Example 2, by mass percentage, consists of the following raw materials: N-octadecyl-1,3-propanediamine 3.6%, ammonium molybdate 4.3%, sodium lysine 2.9%, hydroxyethylidene diphosphonic acid 0.9%, polyoxyethylene sorbitan monostearate 1.3%, and water as the balance.

[0071] Comparative Example 3 The preparation method of the desulfurizing agent for oil and gas field production described in Comparative Example 3 is the same as that in Example 1, except that the raw material composition is different. The desulfurizing agent for oil and gas field production described in Comparative Example 3, by mass percentage, consists of the following raw materials: 3.6% N-octadecyl-1,3-propanediamine, 14% ionic liquid@organic copper mixture, 2.9% sodium lysine, 0.9% hydroxyethylidene diphosphonic acid, 1.3% polyoxyethylene sorbitan monostearate, and water as the balance; wherein, the preparation method of the ionic liquid@organic copper mixture is as follows: first, 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is dried under vacuum, and after the vacuum is stopped, copper naphthenate is added to it under nitrogen protection and stirred at room temperature. After cooling to room temperature, the ionic liquid@organic copper mixture is obtained.

[0072] In the preparation method of the ionic liquid@organic copper mixture, the vacuum drying temperature is 80℃, the vacuum drying pressure is -0.09MPa, and the vacuum drying time is 58min.

[0073] In the preparation method of ionic liquid@organic copper mixture, the stirring speed is 100 r / min and the stirring time is 15 min.

[0074] In the preparation method of ionic liquid@organic copper mixture, the mass ratio of copper naphthenate to 1-butylsulfonic acid-3-methylimidazolium hydrogen sulfate is 1:1.5.

[0075] The desulfurization performance of the desulfurizing agents prepared in Examples 1-3 and Comparative Examples 1-3 was tested below: (1) Hydrogen sulfide gas removal performance test: The desulfurizing agents provided in Examples 1-3 and Comparative Examples 1-3 were used to test the desulfurization performance of the desulfurizing agents at a concentration of 8000 mg / m³. 3 The hydrogen sulfide gas was tested for removal. The desulfurization rate % = (total mass of inlet hydrogen sulfide - total mass of outlet hydrogen sulfide) / total mass of inlet and outlet hydrogen sulfide. The concentration of outlet hydrogen sulfide was recorded. The test results are shown in Table 1 below. (2) Desulfurization performance test during actual oil and gas field development: The daily production of the oil well is 26m³. 3 The wellhead temperature was 55℃, the hydrogen sulfide concentration before treatment was 1000ppm, the methanethiol concentration before treatment was 25ppm, and the carbonyl sulfide concentration before treatment was 15ppm. The desulfurizing agents provided in Examples 1-3 and Comparative Examples 1-3 (the amount of desulfurizing agent used in Examples 1-3 and Comparative Examples 1-3 was 15kg / d) were used for the same duration (30min). The test results after treatment are shown in Table 2 below.

[0076] Table 1 Desulfurization rate test results Table 2. Results of removal of hydrogen sulfide, methanethiol, and carbonyl sulfide As shown in Tables 1 and 2, the desulfurization effect of the desulfurizing agents for oil and gas field production prepared in Examples 1-3 is significantly better than that of Comparative Examples 1-3. The desulfurizing agents for oil and gas field production prepared in Comparative Examples 1-3 have a reduced removal effect on inorganic and organic sulfur due to the absence of any one of the main desulfurization components N-octadecyl-1,3-propanediamine, ionic liquid@organic copper mixture, and ammonium molybdate.

[0077] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A desulfurizing agent for oil and gas field production, characterized in that: By mass percent, consisting of: N-octadecyl-1, 3-propylenediamine 3.5-3.7%, ionic liquid @ organic copper mixture 13-15%, ammonium molybdate 4.0-4.5%, sodium lysine 2.7-3.3%, hydroxy ethylene diphosphonic acid 0.8-1.0%, polyoxyethylene sorbitan monostearate 1.0-1.5%, water as the balance; wherein, the preparation method of the ionic liquid @ organic copper mixture is: first, 1-butyl sulfonic acid-3-methyl imidazole hydrogen sulfate is vacuum dried, after stopping vacuum, under nitrogen protection, copper naphthenate is added to it, stirring reaction is carried out at room temperature, cooling to room temperature to prepare ionic liquid @ organic copper mixture.

2. The oil and gas field oil production desulfurizer according to claim 1, characterized by: The vacuum drying temperature in the preparation method of the ionic liquid @ organic copper mixture is 80℃, the vacuum drying pressure is-0.09MPa, and the vacuum drying time is 55-60min.

3. The oil and gas field produced oil desulfurizer according to claim 1, characterized by: The stirring speed in the preparation method of the ionic liquid @ organic copper mixture is 100r / min, and the stirring time is 15min.

4. The oil and gas field produced oil desulfurizer according to claim 1, characterized by: The mass ratio of copper naphthenate to 1-butyl sulfonic acid-3-methyl imidazole hydrogen sulfate in the preparation method of the ionic liquid @ organic copper mixture is 1:1.

5.

5. A method for preparing the desulfurizing agent for oil and gas field production as described in claim 1, characterized in that: Composed of the following steps: (1) add ionic liquid @ organic copper mixture to the reaction device, heat to 40-42℃ and stir to dissolve; (2) add N-octadecyl-1, 3-propylenediamine, heat to 50-52℃ and continue to stir until the solution is uniform; (3) add hydroxy ethylene diphosphonic acid and stir until completely dispersed; (4) add ammonium molybdate to the reaction system of step (3) in three times, each time interval 5min, and stir evenly; (5) add sodium lysine and stir evenly, then add polyoxyethylene sorbitan monostearate, heat to 54-56℃ and continue to stir evenly, finally add deionized water and stir evenly, vacuum degassing to prepare the desulfurizing agent for oil and gas field oil production.

6. The method for preparing a desulfurizer for oil and gas fields according to claim 5, characterized by: The stirring speed in step (1) is 100r / min, and the stirring time is 10-15min; The stirring speed in step (2) is 100r / min, and the stirring time is 10-15min.

7. The method for preparing a desulfurizer for oil and gas fields according to claim 5, characterized by: The stirring speed in step (3) is 150r / min, and the stirring time is 5-7min.

8. The method for preparing a desulfurizer for oil and gas fields according to claim 5, characterized by: The mass of ammonium molybdate added in step (4) is equal each time, and after three times of addition, continue to stir for 15min; The stirring speed in step (4) is 150r / min.

9. The method for preparing a desulfurizer for oil and gas field production according to claim 5, characterized by: In step (5), add sodium lysine and stir for 5-7min, the stirring speed is 200r / min, add polyoxyethylene sorbitan monostearate and stir for 10-13min, the stirring speed is 200r / min, finally add deionized water and stir for 12-15min, the stirring speed is 200r / min, the vacuum degassing pressure is-0.09MPa, the vacuum degassing time is 10min, and the stirring speed during vacuum degassing is 50r / min.

10. The method for preparing a desulfurizer for oil and gas field production according to claim 5, characterized by: In step (5), when deionized water is added, first preheat the deionized water to 43-45℃ and then add it uniformly.

Citation Information

Patent Citations

  • Preparation method of functionalized polyacid-type sulfonic ionic liquid

    CN102442951A

  • Method for removing thiophene sulfides in fuel oil by catalytic oxidation extraction

    CN102977911A

  • Method for constructing multi-acid-group porous polyion liquid by anion exchange method and application of multi-acid-group porous polyion liquid

    CN115518687A

  • Preparation method and application of cellulose-based polyion liquid polyacid desulfurization catalyst

    CN116196974A

  • Dry fine desulfurization process

    CN116656402A