A desulfurizer main agent, a preparation method thereof, a desulfurizer prepared by the method and application of the desulfurizer

By synthesizing dimethylaminoethyl acrylate and allyl polyoxyethylene ether, and combining suitable reaction conditions and excipients, a desulfurizing agent with high efficiency at high temperatures was prepared, which solved the problem of low desulfurization efficiency of existing technologies under high temperature conditions and achieved efficient and stable removal and inhibition of hydrogen sulfide.

CN121021738BActive Publication Date: 2026-05-19DESHI ENERGY TECH GRP CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
DESHI ENERGY TECH GRP CO LTD
Filing Date
2025-10-27
Publication Date
2026-05-19

AI Technical Summary

Technical Problem

Existing desulfurizing agents are inefficient when used under high temperature conditions (>100℃), making it difficult to meet the mining needs of high-temperature well bottoms, and they cannot effectively inhibit the generation of hydrogen sulfide.

Method used

Using dimethylaminoethyl acrylate and allyl polyoxyethylene ether as the main monomers, a high-temperature resistant desulfurizing agent was prepared by controlling the reaction temperature and time. An auxiliary agent, such as dodecyl dimethyl benzyl ammonium chloride, was added to inhibit the generation of hydrogen sulfide.

Benefits of technology

The prepared desulfurizing agent maintains high desulfurization performance at 130℃, has good chemical stability and rapid hydrogen sulfide absorption capacity, and also has bactericidal effect, making it suitable for desulfurization operations at high-temperature well bottoms.

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Abstract

The application discloses a desulfurizer main agent and a preparation method thereof, a desulfurizer prepared by the method and application of the desulfurizer, and belongs to the technical field of oil exploitation. The desulfurizer is obtained by compounding a main agent and an auxiliary agent according to a mass ratio of (10-15):1, and the main agent has a structure as shown in formula (I). In the formula (I), n is an integer selected from 5-20, and a and b are integers selected from 10-30. The preparation method of the desulfurizer is simple, raw materials are easy to obtain, and the desulfurizer is easy to be industrially produced. The temperature resistance of the desulfurizer can reach 130 DEG C, the desulfurizer has the characteristics of high desulfurization rate and temperature resistance, and is suitable for desulfurization operation of high-temperature wells.
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Description

Technical Field

[0001] This application relates to a desulfurizing agent main agent and its preparation method, the desulfurizing agent obtained therefrom and its application, belonging to the field of petroleum extraction technology. Background Technology

[0002] Currently, numerous high-sulfur oil and gas wells have been developed, significantly impacting crude oil extraction, transportation, and application. Hydrogen sulfide is a highly toxic and irritating gas that not only harms human health and pollutes the environment but also severely corrodes transportation pipelines and related equipment. These issues have become major challenges in crude oil processing and utilization. Furthermore, the escape of hydrogen sulfide during transportation poses dangers to workers and can lead to catalyst poisoning in subsequent crude oil processing units. Therefore, it is essential that hydrogen sulfide in crude oil be removed to below safe concentrations before storage and transportation.

[0003] Currently, the most commonly used desulfurizing agents on the market are triazine desulfurizing agents. Triazine compounds are the most widely used liquid desulfurizing agents, especially water-soluble triazine. Not only does it react rapidly with hydrogen sulfide and have high desulfurization efficiency, but it also has the characteristics of being able to be directly injected into pipelines for desulfurization, being easy to operate, inexpensive and readily available, and having easy-to-remove products. It is particularly suitable for desulfurization in oil and gas fields with low hydrogen sulfide content.

[0004] However, triazine desulfurizers cannot be used at excessively high temperatures; they typically begin to decompose above 85°C, thus affecting desulfurization efficiency. Patent CN107418641A discloses a high-temperature resistant desulfurizer for oil and gas fields and its preparation method, obtained by mixing triazine compounds, organophosphonic acids, heterocyclic organic amines, water-soluble imidazoline, and water, but its temperature resistance is only 90°C. Patent CN113150760A discloses a novel high-temperature resistant desulfurizer and its preparation method, obtained by mixing methyldiethanolamine, monoethanolamine, and hydroxyethyl ethylenediamine, and then reacting it with paraformaldehyde, but its temperature resistance is only 70°C. Therefore, for the exploitation of sulfur-containing oil and gas wells with high bottom-hole temperatures (>100°C), a more temperature-resistant desulfurizer needs to be selected. Summary of the Invention

[0005] To address the aforementioned issues, a method for preparing a desulfurizing agent is provided. The desulfurizing agent prepared by this method can withstand temperatures up to 130°C and still exhibits efficient desulfurization even at high temperatures, enabling desulfurization operations to be performed at high-temperature well bottoms (>100°C).

[0006] According to one aspect of this application, a desulfurizing agent main agent is provided, having a structure as shown in formula (I):

[0007]

[0008] Formula (I)

[0009] Where n is selected from any integer between 5 and 20, and a and b are both selected from any integer between 10 and 30.

[0010] According to another aspect of this application, this application provides a method for preparing a desulfurizing agent, comprising the following steps:

[0011] (1) Mix dimethylaminoethyl acrylate, allyl polyoxyethylene ether and solvent in a mass ratio of 1:(1-5):(3-4.5), add an initiator, and heat to 70-90℃ for 3-5 hours to form a solution containing polymer.

[0012] (2) Remove the solvent from the solution containing the polymer and purify it to obtain the final product.

[0013] Specifically, this application uses dimethylaminoethyl acrylate as the main monomer for the desulfurizing agent. Its structure contains a tertiary amine structure. Due to the absence of active H atoms in its molecule, it has good chemical stability, high selective absorption of hydrogen sulfide, and fast absorption rate.

[0014] In the above structural formula, the tertiary amine group has two methyl groups at its end. The small size of the methyl groups makes it easier for the nitrogen atom of the amine group to contact and react with H₂S or CO₂. In contrast, larger alkyl groups such as ethyl and propyl introduce greater steric hindrance, reducing the collision efficiency between the amine and acidic gas molecules, thus decreasing the reaction rate and absorption capacity. Meanwhile, dimethylaminoethyl acrylate contains an ester group, which, compared to alkyl groups, can exhibit polarity with organosulfur compounds (such as thiophene and benzothiophene). The ester group itself is a polar functional group, and desulfurizers with ester groups can more effectively attract and surround these sulfide molecules through dipole-dipole interactions.

[0015] Specifically, this application uses allyl polyoxyethylene ether, a monomer with a polyoxyethylene ether structure, as another synthetic monomer of the desulfurizing agent, which plays a role in the rapid dispersion of the product, reduces the interfacial tension between the desulfurizing agent and the dispersion medium, makes the desulfurizing agent more wettable, and achieves rapid desulfurization.

[0016] Specifically, this application specifies that the mass ratio of dimethylaminoethyl acrylate to allyl polyoxyethylene ether is 1:(1-5). Under this mass ratio, a desulfurizing agent with a structure of formula (I) with a value of 10-30 for both a and b can be obtained. If the amount of dimethylaminoethyl acrylate added is too small, it will be consumed prematurely, and subsequent chain growth can only be carried out by allyl polyoxyethylene ether, which may make chain termination reaction more likely, resulting in the molecular weight not reaching the expected value. If the amount of dimethylaminoethyl acrylate added is too large, the excess dimethylaminoethyl acrylate may continue to undergo homopolymerization under the action of an initiator after the allyl polyoxyethylene ether is consumed, generating dimethylaminoethyl acrylate homopolymer.

[0017] Specifically, this application specifies the synthesis temperature and time of the main desulfurizing agent. If the reaction temperature is too high, the allyl polyoxyethylene ether will reach its boiling point and boil violently or even splash, causing a safety accident. At the same time, it will also increase the decomposition rate of the initiator, affecting the synthesis effect of the main agent. If the reaction temperature is too low, the reaction rate will be slow, the polymerization efficiency will be low, and a large number of monomers will remain in the product, thus affecting the desulfurization effect of the desulfurizing agent. If the reaction time is too short, a large number of monomers will not participate in the reaction. If the reaction time is too long, it will lead to over-reaction and aggravate the side reactions. All of these will affect the degree of polymerization and purity of the main agent, thereby affecting the desulfurization efficiency of the desulfurizing agent.

[0018] Optionally, the degree of polymerization of the allyl polyoxyethylene ether in step (1) is 5-20.

[0019] Specifically, this application specifies the degree of polymerization of allyl polyoxyethylene ether. When the degree of polymerization of allyl polyoxyethylene ether is 5-20, the polyoxyethylene chain segments are shorter, the molecular volume is smaller, the steric hindrance is lower, the allyl double bonds are fully exposed, and it is easy to contact the double bonds of dimethylaminoethyl acrylate. The polymerization activity is high, it can participate in the polymerization reaction quickly, the reaction conversion rate is high, and the purity of the desulfurizing agent is high. However, when the degree of polymerization is higher (n>20), the polyoxyethylene chain segments become significantly longer, the steric hindrance is greatly increased, resulting in a decrease in polymerization activity, thereby affecting the desulfurization effect of the desulfurizing agent.

[0020] Optionally, the initiator in step (1) is selected from at least one of benzoyl peroxide, lauroyl peroxide, azobisisobutyronitrile, and azobisisoheptanenitrile.

[0021] Optionally, the solvent is selected from at least one of xylene, 100# solvent oil, and 150# solvent oil.

[0022] Optionally, the purification operation in step (2) is as follows: after the polymer has been desolventized, it is dissolved in a solvent again and then the solvent is removed by vacuum decompression. This operation is repeated three times.

[0023] Specifically, this application reduces impurities in the polymer of the desulfurizing agent through purification, while also avoiding the introduction of other impurities, thereby preventing impurities from affecting the desulfurization effect of the desulfurizing agent.

[0024] According to another aspect of this application, this application provides a desulfurizing agent comprising a main agent and an auxiliary agent in a mass ratio of (10-15):1;

[0025] The main agent is selected from the above-mentioned desulfurizing agent main agent or the desulfurizing agent main agent prepared by the above-mentioned preparation method;

[0026] The excipient is selected from at least one of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride, hexadecyl dimethyl benzyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, tetradecyl dimethyl benzyl ammonium bromide, and hexadecyl dimethyl benzyl ammonium bromide.

[0027] Specifically, this application specifies a mass ratio of main agent to excipient of (10-15):1. Since the excipient can only inhibit hydrogen sulfide generated by the reduction reaction of SRB bacteria, it cannot remove already generated hydrogen sulfide. Therefore, increasing the amount of excipient will not only fail to improve desulfurization but will also reduce the proportion of the main agent, thus decreasing the desulfurization rate. If the amount of excipient added is too small, the minimum inhibitory concentration (MIC) required to kill the bacteria cannot be reached. SRB bacteria will only be slightly inhibited or temporarily inhibited, and will then quickly regain activity and continue to reduce sulfate to hydrogen sulfide. The H2S content of the desulfurization system cannot be reduced to the target value, resulting in reduced treatment efficiency.

[0028] Optionally, the preparation method is as follows: the excipient and the main agent are compounded in a certain proportion to obtain the product.

[0029] Optionally, the desulfurizing agent has a temperature resistance of 130°C or higher.

[0030] According to another aspect of this application, this application also provides the application of the above-mentioned desulfurizing agent main agent or the desulfurizing agent main agent prepared by the above-mentioned preparation method or the above-mentioned desulfurizing agent in oil and gas well development.

[0031] The beneficial effects of this application include, but are not limited to:

[0032] 1. The desulfurizing agent main agent according to this application is a polymer-type product with high temperature resistance. When used in a high-temperature environment, the product does not decompose or undergo other side reactions, and still has high selectivity for hydrogen sulfide.

[0033] 2. According to the preparation method of the desulfurizing agent main agent of this application, dimethylaminoethyl acrylate is used as the synthetic monomer of the desulfurizing agent. The amine in its structure is a tertiary amine structure. Since there are no active H atoms in its molecule, it has good chemical stability, high selective absorption of hydrogen sulfide and fast absorption rate.

[0034] 3. According to the preparation method of the desulfurizing agent main agent of this application, allyl polyoxyethylene ether with polyoxyethylene ether structure monomer is used as another synthetic monomer of the desulfurizing agent main agent, which plays a role in rapid dispersion of the product, can reduce the interfacial tension between the desulfurizing agent and the dispersion medium, make the desulfurizing agent more wettable, and achieve rapid desulfurization.

[0035] 4. The desulfurizing agent according to this application uses an auxiliary component with bactericidal effect, which has a highly effective bactericidal effect on SRB bacteria in oil wells. During the oil extraction process, crude oil is mainly a mixture of oil and water. The water part contains a large amount of sulfate ions. When these ions come into contact with SRB bacteria in the soil of the oil extraction formation, hydrogen sulfide gas will be generated under special conditions. The compounded auxiliary agent in this application can inhibit the generation of hydrogen sulfide by eliminating SRB bacteria.

[0036] 5. The desulfurizing agent according to this application has a simple preparation method, readily available raw materials, and is easy to industrialize. It has the characteristics of high desulfurization rate and temperature resistance, and is suitable for desulfurization operations in high-temperature wells.

[0037] 6. The desulfurizing agent according to this application has good regeneration performance. After multiple desulfurization-regeneration cycles, it can still maintain high desulfurization efficiency and sulfur capacity, and its performance decays slowly, which significantly reduces long-term operating costs. Attached Figure Description

[0038] The accompanying drawings, which are included to provide a further understanding of this application and form part of this application, illustrate exemplary embodiments of this application and are used to explain this application, but do not constitute an undue limitation of this application. In the drawings:

[0039] Figure 1 The infrared spectrum of the polymer product of dimethylaminoethyl acrylate and allyl polyoxyethylene ether (n=10) is shown in Example 1 of this application.

[0040] Figure 2 The diagram shows the hydrogen sulfide detection tubes for the blank sample and the sample containing the desulfurizing agent from Example 1. Detailed Implementation

[0041] The present application is described in detail below with reference to the embodiments, but the present application is not limited to these embodiments.

[0042] Unless otherwise specified, the raw materials used in the embodiments and comparative examples of this application were all purchased commercially.

[0043] Unless otherwise specified, the methods used in the embodiments and comparative examples of this application are conventional methods in the prior art.

[0044] Example 1

[0045] A method for preparing a desulfurizing agent, comprising:

[0046] (1) Add 100g of dimethylaminoethyl acrylate, 200g of allyl polyoxyethylene ether (n=10), and 300g of xylene to a three-necked flask and heat and stir until the temperature reaches 90℃. Add 3g of benzoyl peroxide in 5 portions (0.6g each time, with an interval of 10min between each addition). After the addition is complete, keep the mixture at 90℃ for 4.5h to form a polymer. The reaction equation is as follows:

[0047]

[0048] Where: a=20, b=12

[0049] (2) Heat the polymer from step (1) to 150°C, vacuum depressurize for 1 hour to remove the solvent, dissolve the polymer after solvent removal in xylene again, vacuum depressurize for 1 hour to remove the solvent, repeat the operation three times to obtain the main desulfurizing agent.

[0050] (3) Add 25g of dodecyl dimethyl benzyl ammonium chloride to the desulfurizing agent in step (2) and stir for 20min until uniform to obtain desulfurizing agent 1#.

[0051] The desulfurizing agent main agent prepared in Example 1 was subjected to infrared spectroscopy testing, and the test results are shown in the figure. Figure 1 .

[0052] Depend on Figure 1 It can be seen that 1100cm -1 The peak represents the ether bond, at 3500 cm⁻¹. -1 and 1260cm -1 These are the stretching vibration peak of -OH and the in-plane deformation vibration peak, respectively, which are characteristic peaks of ether bonds and hydroxyl groups in allyl polyoxyethylene ether; 3500 cm⁻¹ -1 The peak is a tertiary amine, at 1690 cm⁻¹. -1 The peak represents the ester group, a characteristic peak of the tertiary amine and ester group in dimethylaminoethyl acrylate; 2900 cm⁻¹ -1 The peak is for the methylene group, at 1450 cm⁻¹. -1 The presence of methyl and methylene peaks indicates the occurrence of the polymerization reaction.

[0053] Example 2

[0054] A method for preparing a desulfurizing agent, comprising:

[0055] (1) Add 100g of dimethylaminoethyl acrylate, 250g of allyl polyoxyethylene ether (n=5), and 350g of 100# solvent oil to a three-necked flask and heat and stir until the temperature reaches 90℃. Add 3.5g of lauroyl peroxide in 5 portions (0.7g each time, with an interval of 10min between each addition). After the addition is complete, keep the mixture at 90℃ for 4.5h to form a polymer. The reaction equation is as follows:

[0056]

[0057] Where: a=22, b=28

[0058] (2) Heat the polymer from step (1) to 150°C, vacuum depressurize for 1 hour to remove the solvent, dissolve the polymer after solvent removal in 100# solvent oil again, vacuum depressurize for 1 hour to remove the solvent, repeat the operation three times to obtain the desulfurizing agent main agent.

[0059] (3) Add 30g of tetradecyl dimethyl benzyl ammonium chloride to the desulfurizing agent in step (2) and stir for 20min until uniform to obtain desulfurizing agent 2#.

[0060] Example 3

[0061] A method for preparing a desulfurizing agent, comprising:

[0062] (1) Add 100g of dimethylaminoethyl acrylate, 300g of allyl polyoxyethylene ether (n=15) and 400g of 150# solvent oil to a three-necked flask and heat and stir. Heat to 90℃ and add 4g of azobisisobutyronitrile in 5 portions (0.8g each time, with an interval of 10min between each portion). After the addition is complete, keep the mixture at 90℃ for 4.5h to form a polymer. The reaction equation is as follows.

[0063]

[0064] Where: a=25, b=15

[0065] (2) Heat the polymer from step (1) to 150°C, vacuum depressurize for 1 hour to remove the solvent, dissolve the polymer after solvent removal in 150# solvent oil again, vacuum depressurize for 1 hour to remove the solvent, repeat the operation three times to obtain the desulfurizing agent main agent.

[0066] (3) Add 28g of hexadecyl dimethyl benzyl ammonium chloride to the desulfurizing agent in step (2) and stir for 20min until uniform to obtain desulfurizing agent 3#.

[0067] Example 4

[0068] A method for preparing a desulfurizing agent, comprising:

[0069] (1) Add 100g of dimethylaminoethyl acrylate, 350g of allyl polyoxyethylene ether (n=20) and 450g of xylene to a three-necked flask and heat and stir. Heat to 90℃ and add 4.5g of azobisisoheptanenitrile in 5 portions (0.9g each time, with an interval of 10min between each portion). After the addition is complete, keep the mixture at 90℃ for 4.5h to form a polymer. The reaction equation is as follows.

[0070]

[0071] Where: a=20, b=11

[0072] (2) Heat the polymer from step (1) to 150°C, vacuum depressurize for 1 hour to remove the solvent, dissolve the polymer after solvent removal in xylene again, vacuum depressurize for 1 hour to remove the solvent, repeat the operation three times to obtain the main desulfurizing agent.

[0073] (3) Add 38g of dodecyl dimethyl benzyl ammonium bromide to the desulfurizing agent in step (2) and stir for 20min until uniform to obtain desulfurizing agent 4#.

[0074] Example 5

[0075] A method for preparing a desulfurizing agent, comprising:

[0076] (1) Add 100g of dimethylaminoethyl acrylate, 100g of allyl polyoxyethylene ether (n=10), and 300g of xylene to a three-necked flask and heat and stir. Heat to 80℃, and add 2g of benzoyl peroxide in 5 portions (0.6g each time, with an interval of 10min between each addition). After the addition is complete, keep the mixture at 80℃ for 3h to form a polymer. The reaction equation is as follows:

[0077] Where: a=28, b=10

[0078] (2) Heat the polymer from step (1) to 150°C, vacuum depressurize for 1 hour to remove the solvent, dissolve the polymer after solvent removal in xylene again, vacuum depressurize for 1 hour to remove the solvent, repeat the operation three times to obtain the main desulfurizing agent.

[0079] (3) Add 20g of tetradecyl dimethyl benzyl ammonium bromide to the desulfurizing agent in step (2) and stir for 20min until uniform to obtain desulfurizing agent 5#.

[0080] Example 6

[0081] A method for preparing a desulfurizing agent, comprising:

[0082] (1) Add 100g of dimethylaminoethyl acrylate, 500g of allyl polyoxyethylene ether (n=5), and 350g of 100# solvent oil to a three-necked flask and heat and stir. When the temperature reaches 70℃, add 6g of lauroyl peroxide in 5 portions (0.7g each time, with an interval of 10min between each addition). After the addition is complete, keep the mixture at 90℃ for 5h to form a polymer. The reaction equation is as follows:

[0083]

[0084] Where: a=12, b=30

[0085] (2) Heat the polymer from step (1) to 150°C, vacuum depressurize for 1 hour to remove the solvent, dissolve the polymer after solvent removal in 100# solvent oil again, vacuum depressurize for 1 hour to remove the solvent, repeat the operation three times to obtain the desulfurizing agent main agent.

[0086] (3) Add 40g of hexadecyl dimethyl benzyl ammonium bromide to the desulfurizing agent in step (2) and stir for 20min until uniform to obtain desulfurizing agent 6#.

[0087] Comparative Example 1

[0088] The difference between Comparative Example 1 and Example 1 is that in step (1), allyl polyoxyethylene ether (n=30) is used instead of allyl polyoxyethylene ether (n=10), and the rest are the same.

[0089] Comparative Example 2

[0090] The difference between Comparative Example 2 and Example 1 is that in step (3), the amount of dodecyl dimethyl benzyl ammonium chloride added is 40g, and the rest are the same.

[0091] Comparative Example 3

[0092] The difference between Comparative Example 3 and Example 1 is that in step (1), acrylate is used instead of dimethylaminoethyl acrylate, while the rest are the same.

[0093] Comparative Example 4

[0094] The difference between Comparative Example 4 and Example 1 is that in step (1), diethylaminoethyl acrylate is used instead of dimethylaminoethyl acrylate, while the rest are the same.

[0095] Comparative Example 5

[0096] The difference between Comparative Example 5 and Example 1 is that in step (1), vinyl polyoxyethylene ether-10 is used instead of allyl polyoxyethylene ether (n=10), and the rest are the same.

[0097] Test Example 1: Desulfurization Experiment with Desulfurizing Agent

[0098] Desulfurization comparative experiments were conducted on the desulfurizing agents obtained in the above examples and comparative examples, as well as on 1,3,5-tris(2-hydroxyethyl)-hexahydrotriazine. The desulfurization experiments of the desulfurizing agents were carried out according to the following steps:

[0099] (1) Weigh 1.0g Na2S·9H2O, add 99.0g deionized water, and prepare a 1% sodium sulfide solution for later use.

[0100] (2) Weigh 1.53g of 98% concentrated sulfuric acid into a reagent bottle, add 98.47g of water to prepare a 1.5% dilute sulfuric acid solution for later use.

[0101] (3) Weigh 6.0g of 1% sodium sulfide solution and add it to a 500mL wide-mouth bottle. Then add 100g of deionized water, cover the bottle with a cap that can hold the test tube, and add 100μL of the desulfurizing agent to be tested using a pipette. Shake well. Then add 0.64mL of 1.5% H2SO4 solution, quickly cover the bottle and place it in a 50℃ constant temperature water bath. Shake well and react for 30min. At the same time, perform a blank experiment. The concentration of hydrogen sulfide in the blank sample should be above 600mg / L. Otherwise, repeat the experiment.

[0102] (4) Remove the wide-mouth bottle from the water bath and let it stand for 15 minutes. Then, use a hydrogen sulfide detection tube to measure the concentration of hydrogen sulfide in the wide-mouth bottle. The hydrogen sulfide detection tube should be sealed with the rubber tube with tape to prevent external gas from entering.

[0103] (5) The desulfurization rate is calculated according to formula (1):

[0104] ………………………………(1)

[0105] In the formula:

[0106] X—Desulfurization rate, %

[0107] M0—Measured value of hydrogen sulfide in blank sample, mg / L;

[0108] M1 — The measured value of hydrogen sulfide in the sample of the desulfurizing agent to be tested, in mg / L.

[0109] The test results for each drug are shown in Table 1:

[0110] Table 1 Desulfurization rate data of desulfurizing agents

[0111]

[0112] Depend on Figure 2 The color change indicates that the hydrogen sulfide detected in the sample with the added desulfurizing agent of Example 1 was significantly less than that in the blank sample, indicating that the desulfurizing agent of Example 1 has excellent desulfurization effect.

[0113] As shown in Table 1, the desulfurizers 1#-6# provided in Examples 1-6 have high desulfurization rates, all meeting the industry standard requirement of >90%. Among them, desulfurizer 1# in the examples has the best effect, with 1,3,5-tris(2-hydroxyethyl)-hexahydrotriazine achieving an effect of 97.5%, demonstrating a high desulfurization rate.

[0114] In Comparative Example 1, allyl polyoxyethylene ether with a higher degree of polymerization was used. The excessive proportion of polyoxyethylene in the product structure reduced the desulfurization effect and decreased the desulfurization rate. In Comparative Example 2, increasing the amount of dodecyl dimethyl benzyl ammonium chloride did not achieve better desulfurization. In Comparative Example 3, acrylate without tertiary amine structure was used, and the desulfurization rate of the product decreased significantly. In Comparative Example 4, diethylaminoethyl acrylate was used. The ethyl substituent introduced greater steric hindrance, making the polymerization of the main agent more difficult, resulting in a decrease in the desulfurization rate of the product. In Comparative Example 5, vinyl polyoxyethylene ether-10 was used. The double bond of vinyl is directly connected to the oxygen atom. Its electron cloud density is low, resulting in a significantly lower free radical initiation efficiency than allyl, which affects the polymerization effect of the main agent and leads to poor desulfurization effect of the product.

[0115] Test Example 2: High-Temperature Desulfurization Resistance Experiment of Desulfurizing Agent

[0116] The desulfurizing agents obtained in Examples 1-6 and 1,3,5-tris(2-hydroxyethyl)-hexahydrotriazine were respectively placed in pressure-resistant sealed containers and placed in a muffle furnace for 2 hours. The temperature of the muffle furnace was set to 130°C. After 2 hours, the pressure-resistant sealed containers were removed and cooled. The desulfurization rate of different products was tested according to the desulfurization experiment in Test Example 1 after the products were subjected to high temperature.

[0117] The test results for each drug are shown in Table 2:

[0118] Table 2 Desulfurization rate data of desulfurizing agents

[0119]

[0120] As shown in Table 2, the desulfurization rates of desulfurizing agents 1#-6# after being treated at 130℃ did not decrease at all, proving that they have temperature resistance. However, the desulfurization rate of 1,3,5-tris(2-hydroxyethyl)-hexahydrotriazine decreased to 26.4%, which is a significant decrease and proves that it does not have temperature resistance.

[0121] The above description is merely an embodiment of this application, and the scope of protection of this application is not limited to these specific embodiments, but is determined by the claims of this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the technical concept and principles of this application should be included within the scope of protection of this application.

Claims

1. A desulfurizing agent, characterized in that, Includes a main agent and excipients in a mass ratio of (10-15):1; The main agent has a structure as shown in formula (I): Formula (I) Where n is selected from any integer between 5 and 20, and a and b are both selected from any integer between 10 and 30; The excipient is selected from at least one of dodecyl dimethyl benzyl ammonium chloride, tetradecyl dimethyl benzyl ammonium chloride, hexadecyl dimethyl benzyl ammonium chloride, dodecyl dimethyl benzyl ammonium bromide, tetradecyl dimethyl benzyl ammonium bromide, and hexadecyl dimethyl benzyl ammonium bromide; The method for preparing the desulfurizing agent main component is characterized by comprising the following steps: (1) Mix dimethylaminoethyl acrylate, allyl polyoxyethylene ether and solvent in a mass ratio of 1:(1-5):(3-4.5), add an initiator, and heat to 70-90℃ for 3-5 hours to form a solution containing polymer. (2) Remove the solvent from the solution containing the polymer and purify it to obtain the final product.

2. The desulfurizing agent according to claim 1, characterized in that, The initiator mentioned in step (1) is selected from at least one of benzoyl peroxide, lauroyl peroxide, azobisisobutyronitrile, and azobisisoheptanenitrile.

3. The desulfurizing agent according to claim 1, characterized in that, The solvent mentioned in step (1) is selected from at least one of xylene, 100# solvent oil, and 150# solvent oil.

4. The desulfurizing agent according to claim 1, characterized in that, The purification operation in step (2) is as follows: after the polymer has been desolventized, it is dissolved in a solvent again and then the solvent is removed by vacuum decompression. This operation is repeated three times.

5. The desulfurizing agent according to claim 1, characterized in that, The preparation method is as follows: the excipient and the main agent are compounded in a certain proportion to obtain the product.

6. The desulfurizing agent according to claim 1, characterized in that, The desulfurizing agent has a temperature resistance of over 130℃.

7. The application of the desulfurizing agent according to any one of claims 1-6 in oil and gas well development.