A compound for use as a scale and corrosion inhibitor and a scale and corrosion inhibitor

Abstract

This invention provides a compound for use as a scale and corrosion inhibitor, and a scale and corrosion inhibitor thereof. The compound for use as a scale and corrosion inhibitor has the structure shown in Formula I:

Description

Technical Field

[0001] This invention belongs to the field of oilfield chemical agents, specifically relating to a novel high-temperature resistant water-soluble scale and corrosion inhibitor compound for sulfur-containing gas fields, and a novel high-temperature resistant scale and corrosion inhibitor for sulfur-containing gas fields containing the scale and corrosion inhibitor compound. Background Technology

[0002] In the oil and gas production industry, the presence of components such as H2S, CO2, and inorganic salts can lead to scaling, corrosion, and blockage in oil and gas field gathering and transportation pipelines and wellbores, especially in sulfur-containing gas fields. Sulfur-containing gas fields represent one of the harshest corrosive environments in oil and gas extraction, as highly toxic and corrosive H2S can corrode the metal materials of downhole tubing and surface acquisition and transportation equipment. Measures must be taken to control corrosion and scaling during oil and gas development. With the continuous advancement of oil and gas resource extraction technologies, oil and gas development is progressing towards deeper and ultra-deep formations, with well depths and temperatures constantly reaching new highs, making downhole corrosion control in sulfur-containing gas fields increasingly difficult.

[0003] Adding corrosion inhibitors and scale inhibitors is one of the most common practices, characterized by its simplicity, low cost, and significant effectiveness. However, existing corrosion inhibitors often present several problems when used at high temperatures: firstly, they degrade due to decreased stability; secondly, they desorb due to reduced adsorption between the inhibitor and the metal. The effectiveness of existing corrosion inhibitors typically decreases sharply with increasing temperature, thus they generally fail to meet the required performance at high temperatures.

[0004] In summary, there is a current need to research high-temperature resistant scale and corrosion inhibitors suitable for sulfur-containing gas fields. Summary of the Invention

[0005] The purpose of this invention is to provide a scale and corrosion inhibitor suitable for sulfur-containing gas fields and possessing high-temperature resistance. It exhibits excellent anti-corrosion / scale-forming effects at high temperatures.

[0006] To achieve the above objectives, the present invention provides a compound for scale and corrosion inhibition, having the structure shown in Formula I:

[0007]

[0008] This scale and corrosion inhibitor compound can be applied to sulfur-containing gas field production. It can be quickly adsorbed onto metal surfaces and is not easily degraded at high temperatures, exhibiting excellent anti-corrosion / scale-forming properties at high temperatures.

[0009] According to a specific embodiment of the present invention, preferably, R1 is selected from one of substituted or unsubstituted alkyl groups and aminoalkyl groups; more preferably, R1 is selected from... One of them.

[0010] According to a specific embodiment of the present invention, preferably, R2 is selected from H and substituted or unsubstituted aryl groups; preferably, R2 is selected from... One of them. According to a specific embodiment of the present invention, preferably, R3 is selected from substituted or unsubstituted five- or six-membered rings containing heteroatoms; preferably, R3 is selected from One of them.

[0011] This invention also provides a method for preparing a scale and corrosion inhibitor, which includes the following steps:

[0012] An aldehyde, a polyamine, a ketone, and a first polar solvent are mixed to obtain a first mixture; wherein the molar ratio of the aldehyde, polyamine, and ketone is 1.0-1.2:0.5:1.0-1.2; and the volume of the first polar solvent is 3-5 times the total volume of the aldehyde, polyamine, and ketone.

[0013] After adjusting the pH of the first mixture to 2-6, the first heating reaction was carried out under inert gas protection. The product obtained from the first heating reaction was then purified to remove residual reactants, yielding an intermediate product.

[0014] A second mixture is obtained by mixing a second polar solvent, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product; wherein the mass ratio of the second polar solvent, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product is 100:0.5-1:5-10.

[0015] The second mixture is subjected to a second heating reaction, and the solid precipitate in the product obtained from the second heating reaction is removed, thereby preparing a scale and corrosion inhibitor.

[0016] The method for preparing scale and corrosion inhibitors provided by the present invention can easily and quickly prepare scale and corrosion inhibitors containing compounds having the structure shown in Formula I above.

[0017] According to a specific embodiment of the present invention, preferably, the polyamine includes at least one selected from ethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, and pentaethylenehexamine.

[0018] According to a specific embodiment of the present invention, preferably, the aldehyde includes one of cinnamaldehyde, formaldehyde, and benzaldehyde.

[0019] According to a specific embodiment of the present invention, preferably, the ketone includes one of 2-acetylthiazole, 1-acetylimidazole, and 3-acetylpyridine.

[0020] According to a specific embodiment of the present invention, preferably, the first solvent includes at least one of anhydrous ethanol, deionized water, dimethyl sulfoxide, and N,N-dimethylformamide; more preferably, the first solvent is anhydrous ethanol.

[0021] According to a specific embodiment of the present invention, preferably, the second polar solvent includes at least one of anhydrous ethanol, deionized water, dimethyl sulfoxide, and N,N-dimethylformamide.

[0022] According to a specific embodiment of the present invention, preferably, hydrochloric acid is used as the reagent for pH adjustment of the first mixture; more specifically, the mass concentration of HCl in the hydrochloric acid is 5-20%, based on 100% by mass of the hydrochloric acid.

[0023] According to a specific embodiment of the present invention, preferably, the temperature of the first heating reaction is 70-100°C.

[0024] According to a specific embodiment of the present invention, preferably, the heating reaction time in the first step is 4-10 hours.

[0025] According to a specific embodiment of the present invention, preferably, the temperature of the second heating reaction is 75-95°C.

[0026] According to a specific embodiment of the present invention, preferably, the heating reaction time in the second step is 5-24 hours.

[0027] According to a specific embodiment of the present invention, preferably, the first step of purification treatment of the product obtained by the first heating reaction includes: concentrating the product obtained by the first heating reaction by rotary evaporation until the solvent is completely evaporated, and then removing the remaining reactants by using a third polar solvent and an antisolvent, wherein the volume ratio of the third polar solvent to the antisolvent is 1:2-5.

[0028] More preferably, the temperature for rotary evaporation concentration is 40-70°C;

[0029] More preferably, removing the remaining reactants using a third polar solvent and an antisolvent includes: adding a third polar solvent, then removing the solid precipitate, then adding an antisolvent, mixing with stirring, and then extracting the remaining reactants in an ice bath.

[0030] More preferably, the third polar solvent includes at least one of anhydrous ethanol, deionized water, dimethyl sulfoxide, and N,N-dimethylformamide;

[0031] More preferably, the antisolvent includes at least one of diethyl ether, ethyl acetate, methyl acetate, and acetone;

[0032] More preferably, the mass ratio of the product after rotary evaporation and concentration until the solvent is completely evaporated to the mass of the third polar solvent is 1:5-15.

[0033] According to a specific embodiment of the present invention, preferably, the method further includes:

[0034] The product obtained by removing the solid precipitate from the product obtained by the second heating reaction is mixed with a fourth polar solvent and optional additives to prepare a scale and corrosion inhibitor.

[0035] More preferably, the fourth polar solvent includes at least one of anhydrous ethanol, deionized water, dimethyl sulfoxide, and N,N-dimethylformamide;

[0036] More preferably, the adjuvant includes at least one of potassium iodide, 2-methyl-3-butyn-2-ol, propynyl alcohol, and β-cyclodextrin;

[0037] More preferably, the polar solvent has a mass of 30% or more, based on the mass of the product obtained by removing the solid precipitate from the product obtained by the second heating reaction as 100%.

[0038] More preferably, the mass of the auxiliary agent is 5-15% based on the mass of the product obtained by removing the solid precipitate from the product obtained by the second heating reaction, which is 100%.

[0039] The scale and corrosion inhibitor prepared by the method provided by this invention is water-soluble, suitable for sulfur-containing gas fields, and has excellent high-temperature resistance and anti-corrosion / scale-forming properties.

[0040] The present invention provides a scale and corrosion inhibitor comprising the above-mentioned scale and corrosion inhibitor compound provided by the present invention.

[0041] According to a specific embodiment of the present invention, preferably, the scale inhibitor and corrosion inhibitor further includes a polar solvent;

[0042] More preferably, the polar solvent includes at least one of anhydrous ethanol, deionized water, dimethyl sulfoxide, and N,N-dimethylformamide;

[0043] According to a specific embodiment of the present invention, preferably, the scale inhibitor and corrosion inhibitor further includes an additive;

[0044] More preferably, the adjuvant includes at least one of potassium iodide, 2-methyl-3-butyn-2-ol, propynyl alcohol, and β-cyclodextrin.

[0045] In one specific embodiment of the present invention, a scale and corrosion inhibitor prepared using the above-mentioned method for preparing scale and corrosion inhibitors provided by the present invention is provided.

[0046] The scale and corrosion inhibitor provided by this invention is water-soluble, suitable for sulfur-containing gas fields, and has excellent high-temperature resistance and anti-corrosion / scale properties.

[0047] This invention also provides the application of the above-mentioned scale and corrosion inhibitors in the development of sulfur-containing gas fields.

[0048] According to a specific embodiment of the present invention, preferably, the application environment temperature of the scale and corrosion inhibitor is 0-180℃.

[0049] The scale and corrosion inhibitor compound provided by this invention possesses excellent water solubility, can be rapidly adsorbed onto metal surfaces, and is not easily denatured at high temperatures. The scale and corrosion inhibitor provided by this invention comprises the scale and corrosion inhibitor compound provided by this invention, exhibiting excellent high-temperature resistance and mixed anti-corrosion / scaling effects, effectively protecting against electrochemical corrosion of downhole tubing in sulfur-containing gas fields and reducing scale buildup. Compared with existing technologies, it has the following beneficial effects:

[0050] 1. The scale and corrosion inhibitor provided by the present invention has excellent corrosion inhibition performance and can meet the corrosion inhibition efficiency requirements at extremely low dosages; for example, in some embodiments, the corrosion inhibition efficiency can still reach more than 98% under the conditions of 100 ppm dosage and 80°C.

[0051] 2. The scale and corrosion inhibitor provided by the present invention also has good corrosion inhibition performance under high temperature conditions; for example, in some embodiments, the corrosion inhibition efficiency can still reach more than 93% under the conditions of 1500ppm dosage and 180℃ high temperature.

[0052] 3. The scale inhibitor and corrosion inhibitor provided by the present invention has excellent scale inhibition performance; for example, in some embodiments, the scale inhibition efficiency can reach more than 98% at a dosage of 100 ppm.

[0053] 4. The scale inhibitor and corrosion inhibitor provided by the present invention also have good scale inhibition performance under high temperature conditions; for example, in some embodiments, the scale inhibition efficiency can still reach more than 81% under the conditions of 1500ppm dosage and 180℃ high temperature. Attached Figure Description

[0054] Figure 1 This is the Fourier transform infrared spectrum characterization of the intermediate product in Example 5 of the present invention.

[0055] Figure 2 This is the Fourier transform infrared spectrum characterization of the final product in Example 5 of the present invention.

[0056] Figure 3 This is the nuclear magnetic resonance (NMR) spectrum characterization diagram of the intermediate product in Example 5 of the present invention.

[0057] Figure 4 This is the nuclear magnetic resonance (NMR) spectrum characterization diagram of the final product in Example 5 of the present invention.

[0058] Figure 5 The thermogravimetric analysis diagrams of the final products in Examples 5-8 of this invention are shown. Detailed Implementation

[0059] In order to provide a clearer understanding of the technical features, objectives and beneficial effects of the present invention, the technical solution of the present invention will now be described in detail below, but it should not be construed as limiting the scope of implementation of the present invention.

[0060] Example 1

[0061] This embodiment provides a scale and corrosion inhibitor, the preparation method of which includes the following steps:

[0062] The reactants cinnamaldehyde, diethylenetriamine, and 1-acetylimidazole were added to a reaction vessel in a molar ratio of 1.0:0.5:1.0. Three times the volume of anhydrous ethanol was added to obtain the first mixture. The pH of the first mixture was adjusted to 2 using concentrated hydrochloric acid. Nitrogen gas was continuously introduced into the reaction vessel, and the mixture was heated stably at 70°C for 4 hours to achieve the first heating reaction. After the reaction system cooled, the mixture was concentrated by rotary evaporation at 50°C until the solvent was completely evaporated.

[0063] Anhydrous ethanol (the mass of anhydrous ethanol is 10 times the mass of the product after rotary evaporation and filtration) is added to the product after rotary evaporation and concentration. The solid precipitate is then removed, and ethyl acetate (the volume ratio of anhydrous ethanol to ethyl acetate is 1:5) is added. After stirring and mixing, excess reactants are removed by ice bath extraction to obtain the intermediate product.

[0064] Deionized water, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product were mixed at a mass ratio of 100:0.5:5 to obtain a second mixture. The second mixture was heated stably at 80°C for 5 hours to achieve the second heating reaction. The solid precipitate in the solution was removed by filtration to obtain the final product.

[0065] Adding 40% by weight of deionized water to the final product yields a scale and corrosion inhibitor.

[0066] In the first step of the heating reaction:

[0067]

[0068] In the second step of the heating reaction:

[0069]

[0070] The final product contains a scale and corrosion inhibitor compound with the following structural formula:

[0071]

[0072] Example 2

[0073] This embodiment provides a scale and corrosion inhibitor, the preparation method of which includes the following steps:

[0074] The reactants cinnamaldehyde, tetraethylenepentamine, and 2-acetylthiazol were added to a reaction vessel in a molar ratio of 1.2:0.5:1.1. Three times the volume of anhydrous ethanol was added to obtain the first mixture. The pH of the first mixture was adjusted to 4 using concentrated hydrochloric acid. Nitrogen gas was continuously introduced into the reaction vessel, and the mixture was heated stably at 80°C for 6 hours to achieve the first heating reaction. After the reaction system cooled, the mixture was concentrated by rotary evaporation at 50°C until the solvent was completely evaporated.

[0075] Anhydrous ethanol (the mass of anhydrous ethanol is 10 times the mass of the product after rotary evaporation and filtration) is added to the product after rotary evaporation and concentration. The solid precipitate is then removed, and ethyl acetate (the volume ratio of anhydrous ethanol to ethyl acetate is 1:5) is added. After stirring and mixing, excess reactants are removed by ice bath extraction to obtain the intermediate product.

[0076] Deionized water, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product were mixed at a mass ratio of 100:0.5:10 to obtain a second mixture. The second mixture was heated stably at 80°C for 5 hours to achieve the second heating reaction. The solid precipitate in the solution was removed by filtration to obtain the final product.

[0077] Adding 40% deionized water and 10% potassium iodide by mass of the final product to the final product yields a scale and corrosion inhibitor.

[0078] In the first step of the heating reaction:

[0079]

[0080]

[0081] In the second step of the heating reaction:

[0082]

[0083] The final product contains a scale and corrosion inhibitor compound with the following structural formula:

[0084]

[0085] Example 3

[0086] This embodiment provides a scale and corrosion inhibitor, the preparation method of which includes the following steps:

[0087] The reactants cinnamaldehyde, tetraethylenepentamine, and 2-acetylthiazol were added to a reaction vessel in a molar ratio of 1.0:0.5:1.0. Three times the volume of anhydrous ethanol was added to obtain the first mixture. The pH of the first mixture was adjusted to 6 using concentrated hydrochloric acid. Nitrogen gas was continuously introduced into the reaction vessel, and the mixture was heated stably at 80°C for 8 hours to achieve the first heating reaction. After the reaction system cooled, the mixture was concentrated by rotary evaporation at 50°C until the solvent was completely evaporated.

[0088] Anhydrous ethanol (the mass of anhydrous ethanol is 10 times the mass of the product after rotary evaporation and filtration) is added to the product after rotary evaporation and concentration. The solid precipitate is then removed, and ethyl acetate (the volume ratio of anhydrous ethanol to ethyl acetate is 1:5) is added. After stirring and mixing, excess reactants are removed by ice bath extraction to obtain the intermediate product.

[0089] Deionized water, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product were mixed at a mass ratio of 100:0.5:10 to obtain a second mixture. The second mixture was heated stably at 80°C for 5 hours to achieve the second heating reaction. The solid precipitate in the solution was removed by filtration to obtain the final product.

[0090] Adding 40% deionized water and 10% propargyl alcohol by mass of the final product to the final product yields a scale and corrosion inhibitor.

[0091] In the first step of the heating reaction:

[0092]

[0093]

[0094] In the second step of the heating reaction:

[0095]

[0096] The final product contains a scale and corrosion inhibitor compound with the following structural formula:

[0097]

[0098] Example 4

[0099] This embodiment provides a scale and corrosion inhibitor, the preparation method of which includes the following steps:

[0100] The reactants cinnamaldehyde, tetraethylenepentamine, and 3-acetylpyridine were added to a reaction vessel in a molar ratio of 1.2:0.5:1.1. Three times the volume of anhydrous ethanol was added to obtain the first mixture. The pH of the first mixture was adjusted to 4 using concentrated hydrochloric acid. Nitrogen gas was continuously introduced into the reaction vessel, and the mixture was heated stably at 80°C for 6 hours to achieve the first heating reaction. After the reaction system cooled, the mixture was concentrated by rotary evaporation at 50°C until the solvent was completely evaporated.

[0101] Anhydrous ethanol (the mass of anhydrous ethanol is 10 times the mass of the product after rotary evaporation and filtration) is added to the product after rotary evaporation and concentration. The solid precipitate is then removed, and ethyl acetate (the volume ratio of anhydrous ethanol to ethyl acetate is 1:5) is added. After stirring and mixing, excess reactants are removed by ice bath extraction to obtain the intermediate product.

[0102] Deionized water, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product were mixed at a mass ratio of 100:0.5:10 to obtain a second mixture. The second mixture was heated stably at 90°C for 5 hours to achieve the second heating reaction. The solid precipitate in the solution was removed by filtration to obtain the final product.

[0103] Adding 40% of the final product mass of deionized water and 10% of β-cyclodextrin as an additive to the final product yields a scale and corrosion inhibitor.

[0104] In the first step of the heating reaction:

[0105]

[0106]

[0107] In the second step of the heating reaction:

[0108]

[0109] The final product contains a scale and corrosion inhibitor compound with the following structural formula:

[0110]

[0111] Example 5

[0112] This embodiment provides a scale and corrosion inhibitor, the preparation method of which includes the following steps:

[0113] The reactants cinnamaldehyde, tetraethylenepentamine, and 2-acetylthiazol were added to a reaction vessel in a molar ratio of 1.0:0.5:1.0. Three times the volume of anhydrous ethanol was added to obtain the first mixture. The pH of the first mixture was adjusted to 4 using concentrated hydrochloric acid. Nitrogen gas was continuously introduced into the reaction vessel, and the mixture was heated stably at 80°C for 6 hours to achieve the first heating reaction. After the reaction system cooled, the mixture was concentrated by rotary evaporation at 50°C until the solvent was completely evaporated.

[0114] Anhydrous ethanol (the mass of anhydrous ethanol is 10 times the mass of the product after rotary evaporation and filtration) is added to the product after rotary evaporation and concentration. The solid precipitate is then removed, and ethyl acetate (the volume ratio of anhydrous ethanol to ethyl acetate is 1:5) is added. After stirring and mixing, excess reactants are removed by ice bath extraction to obtain the intermediate product.

[0115] Deionized water, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product were mixed at a mass ratio of 100:0.5:10 to obtain a second mixture. The second mixture was heated stably at 80°C for 5 hours to achieve the second heating reaction. The solid precipitate in the solution was removed by filtration to obtain the final product.

[0116] Adding 40% of the final product mass of deionized water and 10% of β-cyclodextrin as an additive to the final product yields a scale and corrosion inhibitor.

[0117] In the first step of the heating reaction:

[0118]

[0119]

[0120] In the second step of the heating reaction:

[0121]

[0122] The final product contains a scale and corrosion inhibitor compound with the following structural formula:

[0123]

[0124] Example 6

[0125] This embodiment provides a scale and corrosion inhibitor, the preparation method of which includes the following steps:

[0126] The reactants benzaldehyde, tetraethylenepentamine, and 2-acetylthiazol were added to a reaction vessel in a molar ratio of 1.1:0.5:1.1. Three times the volume of anhydrous ethanol was added to obtain the first mixture. The pH of the first mixture was adjusted to 4 using concentrated hydrochloric acid. Nitrogen gas was continuously introduced into the reaction vessel, and the mixture was heated at 75°C for 6 hours to achieve the first heating reaction. After the reaction system cooled, the mixture was concentrated by rotary evaporation at 50°C until the solvent was completely evaporated.

[0127] Anhydrous ethanol (the mass of anhydrous ethanol is 10 times the mass of the product after rotary evaporation and filtration) is added to the product after rotary evaporation and concentration. The solid precipitate is then removed, and ethyl acetate (the volume ratio of anhydrous ethanol to ethyl acetate is 1:3) is added. After stirring and mixing, excess reactants are removed by ice bath extraction to obtain the intermediate product.

[0128] Deionized water, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product were mixed at a mass ratio of 100:0.5:10 to obtain a second mixture. The second mixture was heated stably at 80°C for 5 hours to achieve the second heating reaction. The solid precipitate in the solution was removed by filtration to obtain the final product.

[0129] Add 40% deionized water, 5% propargyl alcohol, and 5% β-cyclodextrin by mass of the final product to the final product to obtain a scale and corrosion inhibitor.

[0130] In the first step of the heating reaction:

[0131]

[0132]

[0133] In the second step of the heating reaction:

[0134]

[0135] The final product contains a scale and corrosion inhibitor compound with the following structural formula:

[0136]

[0137] Example 7

[0138] This embodiment provides a scale and corrosion inhibitor, the preparation method of which includes the following steps:

[0139] Formaldehyde solution (a 37% formaldehyde aqueous solution), tetraethylenepentamine, and 2-acetylthiazole were added to a reaction vessel in a molar ratio of 1.0:0.5:1.0. Three times the volume of anhydrous ethanol was added to obtain the first mixture. The pH of the first mixture was adjusted to 4 using concentrated hydrochloric acid. Nitrogen gas was continuously introduced into the reaction vessel, and the mixture was heated stably at 90°C for 6 hours to achieve the first heating reaction. After the reaction system cooled, the mixture was concentrated by rotary evaporation at 50°C until the solvent was completely evaporated.

[0140] Anhydrous ethanol (the mass of anhydrous ethanol is 10 times the mass of the product after rotary evaporation and filtration) is added to the product after rotary evaporation and concentration. The solid precipitate is then removed, and ethyl acetate (the volume ratio of anhydrous ethanol to ethyl acetate is 1:5) is added. After stirring and mixing, excess reactants are removed by ice bath extraction to obtain the intermediate product.

[0141] Deionized water, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product were mixed at a mass ratio of 100:1:10 to obtain a second mixture. The second mixture was heated stably at 80°C for 5 hours to achieve the second heating reaction. The solid precipitate in the solution was removed by filtration to obtain the final product.

[0142] Add 40% deionized water, 5% potassium iodide, and 5% β-cyclodextrin by mass of the final product to the final product to obtain a scale and corrosion inhibitor.

[0143] In the first step of the heating reaction:

[0144]

[0145] In the second step of the heating reaction:

[0146]

[0147]

[0148] The final product contains a scale and corrosion inhibitor compound with the following structural formula:

[0149]

[0150] Example 8

[0151] This embodiment provides a scale and corrosion inhibitor, the preparation method of which includes the following steps:

[0152] The reactants cinnamaldehyde, tetraethylenepentamine, and 2-acetylthiazol were added to a reaction vessel in a molar ratio of 1.2:0.5:1.2. Three times the volume of anhydrous ethanol was added to obtain the first mixture. The pH of the first mixture was adjusted to 6 using concentrated hydrochloric acid. Nitrogen gas was continuously introduced into the reaction vessel, and the mixture was heated stably at 80°C for 10 hours to achieve the first heating reaction. After the reaction system cooled, the mixture was concentrated by rotary evaporation at 50°C until the solvent was completely evaporated.

[0153] Dimethyl sulfoxide (the mass of anhydrous ethanol is 10 times the mass of the product after rotary evaporation and filtration) was added to the product after rotary evaporation and concentration. The solid precipitate was then removed, and ethyl acetate (the volume ratio of dimethyl sulfoxide to ethyl acetate was 1:5) was added. After stirring and mixing, the product was extracted in an ice bath to remove excess reactants and obtain the intermediate product.

[0154] Dimethyl sulfoxide, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product were mixed at a mass ratio of 100:0.5:10 to obtain a second mixture. The second mixture was heated stably at 80°C for 5 hours to achieve the second heating reaction. The solid precipitate in the solution was removed by filtration to obtain the final product.

[0155] Adding 40% dimethyl sulfoxide, 5% potassium iodide, and 5% β-cyclodextrin by mass of the final product to the final product yields a scale and corrosion inhibitor.

[0156] In the first step of the heating reaction:

[0157]

[0158] In the second step of the heating reaction:

[0159]

[0160]

[0161] The final product contains a scale and corrosion inhibitor compound with the following structural formula:

[0162]

[0163] Example 9

[0164] This embodiment provides a scale and corrosion inhibitor, the preparation method of which includes the following steps:

[0165] The reactants cinnamaldehyde, tetraethylenepentamine, and 2-acetylthiazol were added to a reaction vessel in a molar ratio of 1.2:0.5:1.2. Three times the volume of anhydrous ethanol was added to obtain the first mixture. The pH of the first mixture was adjusted to 6 using concentrated hydrochloric acid. Nitrogen gas was continuously introduced into the reaction vessel, and the mixture was heated stably at 80°C for 10 hours to achieve the first heating reaction. After the reaction system cooled, the mixture was concentrated by rotary evaporation at 50°C until the solvent was completely evaporated.

[0166] Dimethyl sulfoxide (the mass of anhydrous ethanol is 10 times the mass of the product after rotary evaporation and filtration) was added to the product after rotary evaporation and concentration. The solid precipitate was then removed, and ethyl acetate (the volume ratio of dimethyl sulfoxide to ethyl acetate was 1:5) was added. After stirring and mixing, the product was extracted in an ice bath to remove excess reactants and obtain the intermediate product.

[0167] Dimethyl sulfoxide, sodium 2-hydroxy-3-chloropropyl phosphate (HCP), and the intermediate product were mixed at a mass ratio of 100:0.5:10 to obtain a second mixture. The second mixture was heated stably at 80°C for 5 hours to achieve the second heating reaction. The solid precipitate in the solution was removed by filtration to obtain the final product.

[0168] Adding 40% dimethyl sulfoxide, 5% 2-methyl-3-butyn-2-ol, and 5% β-cyclodextrin by mass of the final product to the final product yields a scale and corrosion inhibitor.

[0169] In the first step of the heating reaction:

[0170]

[0171] In the second step of the heating reaction:

[0172]

[0173]

[0174] The final product contains a scale and corrosion inhibitor compound with the following structural formula:

[0175]

[0176] Product performance testing:

[0177] Experimental Example 1:

[0178] The scale inhibitors and corrosion inhibitors provided in Examples 1-8 were tested for corrosion inhibition performance under normal pressure.

[0179] The testing process was as follows: The scale and corrosion inhibitors provided in Examples 1-8 were subjected to corrosion tests on water samples containing H2S and CO2. The corrosion test procedure was performed in accordance with Section 3, "Determination Method of Static Corrosion Rate and Inhibition Rate under Atmospheric Pressure," of the Chinese Petroleum Industry Standard SY / T 5273-2000, "Evaluation Method for Corrosion Inhibitors in Oilfield Produced Water." The test specimens were made of BG110SS seamless steel pipe used in well tubing. The corrosion test medium was an aqueous solution containing 50,000 ppm NaCl, 1,000 ppm H2S, and 300 ppm CO2. The concentration of the scale and corrosion inhibitor was 100 ppm (based on 100% of the total mass of the corrosion test medium). The temperature environment was 80℃, and the oxygen environment was oxygen-free. After 72 hours of corrosion under these conditions, the corrosion rate r was determined based on the difference in specimen mass before and after the test. corr And corrosion inhibition rate η.

[0180] Among them, the annual corrosion rate r corr It is determined by the following formula:

[0181]

[0182] In the formula: r corr The corrosion rate is expressed as millimeters per year (mm / a); Δm is the weight loss of the coupon, expressed as grams (g); and s is the exposed area of ​​the coupon, expressed as square centimeters (cm²). 2 ); t is the experimental time, in hours (h); ρ is the relative density of the hanging tablets, in grams per cubic centimeter (g / cm³). 3 ).

[0183] The corrosion inhibition rate η is determined by the following formula:

[0184]

[0185] In the formula: η is the corrosion inhibition rate, %; Δm0 is the weight loss of the coupon in the blank test, in grams (g); Δm1 is the weight loss of the coupon after adding the corrosion inhibitor, in grams (g).

[0186] The corrosion inhibition rates of samples using the scale and corrosion inhibitors provided in Examples 1-8 were statistically analyzed, and the results are shown in Table 1:

[0187] Table 1

[0188] blank 80 — 1 80 84.7 2 80 97.1 3 80 92.6 4 80 90.4 5 80 97.6 6 80 93.1 7 80 88.2 8 80 98.0 9 80 92.8

[0189] As can be seen from Table 1, the scale and corrosion inhibitor provided by the present invention has excellent corrosion inhibition performance at 80°C, with a corrosion inhibition efficiency of over 80%, and in preferred embodiments, the corrosion inhibition efficiency can reach 98%.

[0190] Experimental Example 2:

[0191] The scale inhibitors and corrosion inhibitors provided in Examples 1-8 were tested for corrosion inhibition performance under high temperature and high pressure.

[0192] The testing process was as follows: The scale and corrosion inhibitors provided in Examples 1-8 were subjected to corrosion tests in high-temperature and high-pressure environments containing H2S and CO2. The corrosion test procedure was performed in accordance with the American Society for Testing and Materials (ASTM) standard G111, "Standard Guide for Corrosion Tests in High Temperature or High Pressure Environment, or Both". The test specimens were made of BG110SS seamless steel pipe, the corrosion test medium was an aqueous solution containing 50,000 ppm NaCl, 1,000 ppm H2S, and 300 ppm CO2, the concentration of the scale and corrosion inhibitor was 1500 ppm (based on 100% of the total mass of the corrosion test medium), the H2S partial pressure was 0.5 MPa, the CO2 partial pressure was 3.0 MPa, the total pressure was 10 MPa, the temperature was 180°C, and the oxygen environment was oxygen-free. After corrosion for 72 hours under the above conditions, the corrosion inhibition rate η was determined according to the method in Example 1.

[0193] The corrosion inhibition rates of samples using the scale and corrosion inhibitors provided in Examples 1-8 under high temperature and high pressure were statistically analyzed, and the results are shown in Table 2:

[0194] Table 2

[0195] blank 180 — 1 180 46.2 2 180 74.8 3 180 76.2 4 180 67.5 5 180 93.3 6 180 82.4 7 180 87.5 8 180 92.5 9 180 79.9

[0196] As can be seen from Table 2, the scale and corrosion inhibitor provided by the present invention has excellent corrosion inhibition performance at a high temperature of 180℃, with a corrosion inhibition efficiency of over 45%, and in preferred embodiments, the corrosion inhibition efficiency can reach over 93%.

[0197] Experimental Example 3:

[0198] The scale inhibition performance of the scale inhibitors and corrosion inhibitors provided in Examples 1-8 was tested.

[0199] The testing process specifically involved evaluating the scale inhibition performance of the scale and corrosion inhibitors provided in Examples 1-8 using static scale inhibition experiments. The static scale inhibition experiment procedure was conducted according to Section A.3.3, "Scale Inhibition Rate of CaCO3 Scale," of China Petroleum Enterprise Standard Q / SY 126-2014, "Technical Specification for Corrosion and Scale Inhibitors for Oilfield Water Treatment." The concentration of the scale and corrosion inhibitor used was 100 ppm, and the calcium ion content was determined using EDTA titration.

[0200] Scale inhibition performance is expressed as scale inhibition rate X (%), and is determined according to the following formula:

[0201]

[0202] In the formula: V1 is the volume of EDTA standard solution consumed after adding scale inhibitor, in milliliters (mL); V0 is the volume of EDTA standard solution consumed in titrating blank sample 1, in milliliters (mL); V is the volume of EDTA standard solution consumed in titrating blank sample 2, in milliliters (mL).

[0203] The scale inhibition rate of samples using the scale and corrosion inhibitors provided in Examples 1-8 was statistically analyzed, and the results are shown in Table 3:

[0204] Table 3

[0205] Blank 1 50 — Two blank samples 50 — 1 50 91.1 2 50 97.4 3 50 96.5 4 50 97.2 5 50 95.3 6 50 98.1 7 50 92.3 8 50 94.6 9 50 95.0

[0206] As can be seen from Table 3, the scale inhibitor and corrosion inhibitor provided by the present invention has excellent scale inhibition performance, with a scale inhibition efficiency of over 90%, and in preferred embodiments, the scale inhibition efficiency can reach over 98%.

[0207] Experimental Example 4:

[0208] The scale inhibition performance of the scale inhibitors and corrosion inhibitors provided in Examples 1-8 was tested at a high temperature of 180°C.

[0209] The testing process specifically involves evaluating the scale inhibition performance of the scale and corrosion inhibitors provided in Examples 1-8 at a high temperature of 180°C using static scale inhibition experiments. The static scale inhibition test procedure was performed in accordance with Section A.3.3, "Scale Inhibition Rate of CaCO3 Scale," of the China Petroleum Enterprise Standard Q / SY 126-2014, "Technical Specification for Corrosion and Scale Inhibitors for Oilfield Water Treatment." Specifically, when performing step a) of section 3.3.1, the following adjustments were made: Take 200 mL of distilled water into a 250 mL volumetric flask, accurately add 6.00 mL of CaCl solution, accurately add 7.5 mL of scale and corrosion inhibitor solution, let stand for 10 minutes, then add 6.00 mL of Na2CO3 solution dropwise while shaking, dilute with distilled water to the mark, shake well, and pour the above solution into a 500 mL hydrothermal reactor. Seal the reactor and place it in a 50℃±1℃ water bath for half an hour until the temperature reaches equilibrium. Afterward, open the cap to release the gas, then tighten the cap again and let it stand in an oven at 180℃±5℃ for 16 hours.

[0210] The concentration of the scale and corrosion inhibitor used was 1500 ppm, and the calcium ion content was determined by EDTA titration.

[0211] Scale inhibition performance is expressed as scale inhibition rate X (%), and is determined according to the following formula:

[0212]

[0213] In the formula: V1 is the volume of EDTA standard solution consumed after adding scale inhibitor, in milliliters (mL); V0 is the volume of EDTA standard solution consumed in titrating blank sample 1, in milliliters (mL); V is the volume of EDTA standard solution consumed in titrating blank sample 2, in milliliters (mL).

[0214] The scale inhibition rate of samples using the scale and corrosion inhibitors provided in Examples 1-8 was statistically analyzed, and the results are shown in Table 4:

[0215] Table 4

[0216] Blank 1 180 — Two blank samples 180 — 1 180 52.1 2 180 71.6 3 180 69.1 4 180 78.2 5 180 79.0 6 180 81.3 7 180 73.3 8 180 78.9 9 180 77.8

[0217] As can be seen from Table 4, the scale inhibitor and corrosion inhibitor provided by the present invention has excellent scale inhibition performance at high temperatures. At 180°C, the scale inhibition efficiency can reach 81.3% in a preferred embodiment.

[0218] Experimental Example 5:

[0219] The intermediate and final products in Example 5 were characterized by Fourier transform infrared spectroscopy and nuclear magnetic resonance spectroscopy, respectively. The results are as follows: Figure 1 , Figure 2 , Figure 3 , Figure 4 As shown.

[0220] Figure 1 The image shows the Fourier transform infrared spectrum of the intermediate product in Example 5. Figure 1 Middle, 1300.15cm -1 1349.97cm -1 1384.29cm -1 The small, sharp absorption peak at 1492.48 cm⁻¹ is attributed to the stretching vibration of the CH bond in the alkyl group. -1 The small, sharp peak is attributed to the deformation vibration of the CN bond, 1598.2 cm⁻¹. -1 The strong absorption peak nearby is attributed to the stretching vibration of NH4+, 762.49 cm2. -1 The absorption peak at 700.61 cm⁻¹ is attributed to the stretching vibration peak of CS. -1 The stretching vibration peak of the carbonyl C=O group is located at 1690 cm⁻¹, attributed to the out-of-plane bending vibration of the phenyl CH bond. -1 -1750cm -1 It merges with the characteristic peak of NH to form a broad and strong peak, 2819.31 cm⁻¹. -1 The broadband absorption band is attributed to the torsional vibration of C=N, 3411.81 cm⁻¹ -1 The broad-band strong absorption band at that point is attributed to the stretching vibration of OH. Figure 3This is the NMR spectrum characterization of the intermediate product in Example 5. Figure 3 In the 1H NMR (DMSO, 400MHz), the proton peak at 1.83ppm is the proton peak of the secondary amine -NH; the chemical shifts at 2.65ppm and 2.67ppm are the proton peaks of the methylene group in -NH-CH2-CH2-NH-; the proton peaks at 7.23ppm-7.31ppm are the proton peaks of the phenyl group; the chemical shifts at 8.14ppm-8.21ppm are the proton peaks of the -CH=CH- group on the thiazole ring; the chemical shift at 6.5ppm is the proton peak of the -CH=CH- group connected to the phenyl group; and the chemical shifts at 3.41ppm-3.45ppm are the proton peaks of the methine group.

[0221] Figure 2 The image shows the Fourier transform infrared spectrum of the final product in Example 5. Figure 2 Middle, 1294.32cm -1 1351.98cm -1 1384.40cm -1 The small, sharp absorption peak at 1493.48 cm⁻¹ is attributed to the stretching vibration of the CH bond in the alkyl group. -1 The small, sharp peak is attributed to the deformation vibration of the CN bond, 1599.38 cm⁻¹. -1 The strong absorption peak nearby is attributed to the stretching vibration of NH4+, 765.14 cm2. -1 The absorption peak at 702.17 cm⁻¹ is attributed to the stretching vibration peak of CS. -1 The stretching vibration peak of the carbonyl C=O group, attributed to the out-of-plane bending vibration of the phenyl CH bond, is located at 1690-1750 cm⁻¹. -1 It merges with the characteristic peak of NH to form a broad and strong peak at 2800 cm⁻¹. -1 The broad absorption band is attributed to the torsional vibration of C=N, which is weakened by the quaternization reaction, resulting in a peak at 3414.56 cm⁻¹. -1 The broad, strong absorption band at this point is attributed to the stretching vibration of the OH group. (1080.84 cm⁻¹) -1 The characteristic absorption peak at 937.24 cm⁻¹ is attributed to the introduction of the P=O stretching vibration. -1 The location is attributed to the introduced POC bending vibration, 873.55 cm. -1 The C-Cl absorption peak at that point is almost invisible, which is attributed to the quaternization reaction leading to the conversion of the C-Cl bond into a CN bond. Figure 4 This is the NMR spectrum characterization of the final product in Example 5. Figure 4In the 1H NMR (DMSO, 400MHz) spectrum, the chemical shift at 1.23 ppm is the proton peak of the -N-CH2-C- group introduced into the HCP; the chemical shift at 1.84 ppm is the proton peak of the secondary amine -NH; the chemical shift at 1.91 ppm is the proton peak of the -OH group introduced into the HCP; the chemical shifts from 2.64 ppm to 2.88 ppm are the proton peaks of the methylene group in -NH-CH2-CH2-NH-; the chemical shifts from 3.01 ppm to 3.38 ppm are the proton peaks of the methine group; the chemical shift at 6.52 ppm is the proton peak of -CH=CH-; the chemical shifts from 7.32 ppm to 7.42 ppm are the proton peaks of the phenyl group; and the chemical shifts from 7.66 ppm to 7.68 ppm are the proton peaks of the -CH=CH- group on the thiazole ring.

[0222] Thermogravimetric analysis was performed on the final products of Examples 5-8, and the results are as follows: Figure 5 As shown. Example 7 showed significant weight loss at 190°C, attributed to the thermal decomposition of the compound, and again at 270°C, attributed to secondary thermal decomposition of the sample; Example 5 showed significant weight loss at 268°C, attributed to the thermal decomposition of the compound; Example 6 showed significant weight loss at 249°C, attributed to the thermal decomposition of the compound; Example 8 showed significant weight loss at 266°C, attributed to the thermal decomposition of the compound. Thermal analysis showed that the final products in Examples 5-8 possessed excellent thermal stability.

[0223] Thus, specific embodiments of the subject matter have been described. Other embodiments are within the scope of the appended claims. In some cases, the actions recited in the claims may be performed in a different order and still achieve the desired result. Furthermore, the processes depicted in the drawings are not necessarily shown in a specific order or sequence to achieve the desired result.

Claims

1. A compound for use as a scale and corrosion inhibitor, having the structure shown in Formula I: Formula I; in, R3 is selected from , , One of them; Wherein, R1 is selected from , , , , , One of them; Wherein, R2 is selected from , , One of them.

2. A method for preparing a scale and corrosion inhibitor comprising the compound of claim 1, comprising the following steps: An aldehyde, a polyamine, a ketone, and a first polar solvent are mixed to obtain a first mixture; wherein the molar ratio of the aldehyde, polyamine, and ketone is 1.0-1.2:0.5:1.0-1.2; and the volume of the first polar solvent is 3-5 times the total volume of the aldehyde, polyamine, and ketone. After adjusting the pH of the first mixture to 2-6, a first-step heating reaction was carried out under inert gas protection. The product obtained from the first-step heating reaction was then subjected to a first-step purification process to remove residual reactants and obtain an intermediate product. The temperature of the first-step heating reaction was 70-100℃. A second mixture is obtained by mixing a second polar solvent, sodium 2-hydroxy-3-chloropropyl phosphate, and the intermediate product; wherein the mass ratio of the second polar solvent, sodium 2-hydroxy-3-chloropropyl phosphate, and the intermediate product is 100:0.5-1:5-10; wherein the temperature of the second heating reaction is 75-95°C. The second mixture is subjected to a second heating reaction, and the solid precipitate in the product obtained from the second heating reaction is removed, thereby preparing a scale and corrosion inhibitor. Among them, ketones include one of 2-acetylthiazole, 1-acetylimidazolium, and 3-acetylpyridine; Among them, polyamines include at least one of ethylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, and pentaethylenehexamine; Aldehydes include one of cinnamaldehyde, formaldehyde, and benzaldehyde.

3. The preparation method according to claim 2, wherein, The first solvent includes at least one of anhydrous ethanol, deionized water, dimethyl sulfoxide, and N,N-dimethylformamide; and / or The second polar solvent includes at least one of anhydrous ethanol, deionized water, dimethyl sulfoxide, and N,N-dimethylformamide.

4. The preparation method according to claim 2, wherein, Hydrochloric acid was used as the reagent for pH adjustment of the first mixture.

5. The preparation method according to claim 4, wherein, Based on the mass of hydrochloric acid as 100%, the mass concentration of HCl in hydrochloric acid is 5-20%.

6. The preparation method according to claim 2, wherein, The first step of the heating reaction takes 4-10 hours.

7. The preparation method according to claim 2, wherein, The second step of the heating reaction takes 5-24 hours.

8. The preparation method according to claim 2, wherein, The first purification process for the product obtained from the first heating reaction includes: concentrating the product obtained from the first heating reaction by rotary evaporation until the solvent is completely evaporated, and then removing the remaining reactants using a third polar solvent and an antisolvent; wherein the volume ratio of the solvent to the antisolvent is 1:2-5.

9. The preparation method according to claim 8, wherein, The third polar solvent includes at least one of anhydrous ethanol, deionized water, dimethyl sulfoxide, and N,N-dimethylformamide.

10. The preparation method according to claim 8, wherein, The antisolvent includes at least one of diethyl ether, ethyl acetate, methyl acetate, and acetone.

11. The preparation method according to claim 8, wherein, The mass ratio of the product after rotary evaporation and concentration until the solvent is completely evaporated to the mass of the third polar solvent is 1:5-15.

12. The preparation method according to claim 8, wherein, The removal of residual reactants using a third polar solvent and an antisolvent involves: adding a third polar solvent, removing the solid precipitate, adding an antisolvent, mixing with stirring, and then extracting the remaining reactants in an ice bath.

13. The preparation method according to claim 2, wherein, The method also includes: The product obtained by removing the solid precipitate from the product obtained by the second heating reaction is mixed with a fourth polar solvent and optional additives to prepare a scale and corrosion inhibitor.

14. The preparation method according to claim 13, wherein, The fourth polar solvent includes at least one of anhydrous ethanol, deionized water, dimethyl sulfoxide, and N,N-dimethylformamide.

15. The preparation method according to claim 13, wherein, The adjuvant includes at least one of potassium iodide, 2-methyl-3-butyn-2-ol, propynyl alcohol, and β-cyclodextrin.

16. The preparation method according to claim 13, wherein, The mass of the polar solvent is 30% or more, based on the mass of the product obtained by removing the solid precipitate from the product obtained by the second heating reaction as 100%.

17. The preparation method according to claim 13, wherein, The mass of the auxiliary agent is 5-15% based on the mass of the product obtained by removing the solid precipitate from the product obtained by the second heating reaction, which is 100%.

18. A scale and corrosion inhibitor comprising the compound for use as described in claim 1.

19. The scale and corrosion inhibitor according to claim 18, wherein, This scale and corrosion inhibitor also includes polar solvents.

20. The scale and corrosion inhibitor according to claim 19, wherein, The polar solvent includes at least one of anhydrous ethanol, deionized water, dimethyl sulfoxide, and N,N-dimethylformamide.

21. The scale and corrosion inhibitor according to claim 18, wherein, This scale and corrosion inhibitor also includes additives; The adjuvant includes at least one of potassium iodide, 2-methyl-3-butyn-2-ol, propynol, and β-cyclodextrin.

22. The scale and corrosion inhibitor according to claim 18, wherein, The scale and corrosion inhibitor is prepared using the method described in any one of claims 2-17.

23. The application of the scale and corrosion inhibitor according to any one of claims 19-22 in the development of sulfur-containing gas fields.

24. The application according to claim 23, wherein, The application environment temperature for scale and corrosion inhibitors is 0-180℃.

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