Solid corrosion-inhibition, scale-inhibition and paraffin-inhibition integrated medicament and preparation method thereof

Abstract

The invention discloses a solid corrosion inhibition, scale inhibition and paraffin inhibition integrated agent and a preparation method thereof, and belongs to the technical field of oilfield chemistry. The preparation method comprises the following steps: carrying out acylation reaction by taking polyacrylic acid and hydroxyethyl ethylenediamine as raw materials to generate an acylated product; carrying out cyclization reaction on the acylated product to generate an imidazoline compound; the preparation method comprises the following steps: carrying out esterification reaction on an imidazoline compound and benzoic acid in the presence of a catalyst to prepare an intermediate product; the preparation method comprises the following steps: reacting epoxy chloropropane and sodium phosphate serving as raw materials to generate a chlorinated phosphating reagent; and carrying out quaternization reaction by taking the intermediate product and a chlorinated phosphating reagent as raw materials to prepare a phosphorus phenyl imidazoline quaternary ammonium salt compound, and concentrating the phosphorus phenyl imidazoline quaternary ammonium salt compound to prepare the medicament. In the agent, an imidazoline quaternary ammonium salt compound prepared by quaternization reaction is an important component for exerting a corrosion inhibition effect, and a phosphate radical group and a phenyl group which are nodular through substitution reaction are important components for exerting scale inhibition and paraffin inhibition effects. The three-proofing solid medicament has very obvious inhibition effects on corrosion, scaling and wax precipitation of metal.

Description

Technical Field

[0001] This invention belongs to the field of oilfield chemical technology, specifically relating to an integrated solid corrosion inhibitor, scale inhibitor, and wax inhibitor and its preparation method. Background Technology

[0002] As oilfield development enters its mid-to-late stages, the production environment of oil wells becomes increasingly severe. Problems such as corrosion, scaling, and wax buildup intertwine, causing serious damage to the wellbore. This manifests as frequent casing perforation, sucker rod jamming due to blockage, and a significant decrease in pump efficiency, directly restricting wellbore lifting efficiency and impacting the overall production benefits of the oilfield. Faced with this challenge, the commonly used strategy in the field is to frequently add various liquid corrosion inhibitors, scale inhibitors, and wax removers to the oil wells. However, this traditional method is not only complex and cumbersome in its operation, increasing manpower and material resources, but also costly and difficult to maintain long-term. Even more problematic is that some oil wells have excessively high gas content, making the smooth injection of liquid agents extremely difficult, further weakening the treatment effect.

[0003] Therefore, given the numerous shortcomings of liquid chemical agents in oil wellbore treatment, it is urgent to develop solid, multifunctional, slow-release, long-acting agents that meet oilfield operating conditions, are easy to use, economical, and efficient. This is also of great significance for enriching the variety of oilfield chemical products for production and transportation. Summary of the Invention

[0004] To overcome the shortcomings of the prior art, the present invention aims to provide a solid corrosion inhibitor, scale inhibitor, and wax inhibitor, and its preparation method. In this agent, the imidazoline quaternary ammonium salt compound prepared by quaternization reaction is a key component for corrosion inhibition, while the phosphate and phenyl groups obtained through substitution reaction are key components for scale inhibition and wax prevention. This three-inhibition solid agent exhibits a highly significant inhibitory effect on metal corrosion, scaling, and wax formation.

[0005] To achieve the above objectives, the present invention employs the following technical solution:

[0006] This invention provides a method for preparing the above-mentioned integrated solid corrosion inhibitor, scale inhibitor, and wax inhibitor, comprising the following steps:

[0007] S1: Using polyacrylic acid and hydroxyethyl ethylenediamine as raw materials, an acylation reaction is carried out to generate an acylated product; the acylated product is then subjected to a cyclization reaction to generate an imidazoline compound;

[0008] S2: An intermediate product is obtained by esterification of imidazoline compound and benzoic acid in the presence of a catalyst.

[0009] S3: Epichlorohydrin and sodium phosphate are reacted to generate a chlorinated phosphating agent; the intermediate product and the chlorinated phosphating agent are used as raw materials to carry out a quaternization reaction to obtain a phosphophenylimidazoline quaternary ammonium salt compound; the phosphophenylimidazoline quaternary ammonium salt compound is concentrated to obtain the reagent.

[0010] In one embodiment, in S1, the mass ratio of polyacrylic acid and hydroxyethyl ethylenediamine is (2-4):1.

[0011] In one embodiment, in S1, the molecular weight of the polyacrylic acid is selected to be 200-600; the reaction temperature of the acylation reaction is 140-170℃, and the reaction time of the acylation reaction is 6h; the reaction temperature of the cyclization reaction is 200-230℃, and the reaction time of the cyclization reaction is 4-6h.

[0012] In one embodiment, in S2, the mass ratio of the imidazoline compound to benzoic acid is (1-1.2):1.

[0013] In one embodiment, in step S2, the catalyst is p-toluenesulfonic acid; the reaction temperature of the esterification reaction is 100-120°C, and the reaction time is 3 hours.

[0014] In one embodiment, in step S3, the mass ratio of epichlorohydrin to sodium phosphate is 1:(1.2-2).

[0015] In one embodiment, the preparation method of the chlorophosphating agent in S3 is as follows: epichlorohydrin and sodium phosphate are reacted in the presence of the catalyst triphenyl phosphate at a controlled temperature of 180-200°C for 2 hours to obtain the chlorophosphating agent.

[0016] In one embodiment, in step S3, the mass ratio of the intermediate product to the chlorinated phosphating agent is 1:1; the temperature of the quaternization reaction is 85-100°C; and the time of the quaternization reaction is 5 hours.

[0017] In one embodiment, the process of obtaining the pharmaceutical agent through concentration in S3 is as follows: the phosphophenylimidazoline quaternary ammonium salt compound is concentrated and mixed, and then integrally molded by pressure injection molding machine to obtain the pharmaceutical agent.

[0018] In another aspect, the present invention provides a solid corrosion inhibitor, scale inhibitor, and wax inhibitor prepared by the above-mentioned method for preparing an integrated solid corrosion inhibitor, scale inhibitor, and wax inhibitor.

[0019] Specifically, the structural formula of the drug is as follows:

[0020]

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] This invention provides a method for preparing a solid corrosion inhibitor, scale inhibitor, and wax inhibitor integrated agent. In this preparation process, a functional group with corrosion inhibition properties is synthesized through acylation, cyclization, and quaternization reactions. A phenyl functional group with wax inhibitor properties is introduced through esterification. A phosphate group with scale inhibition effect is introduced through substitution. Finally, the agent is extruded and granulated to obtain a chemical agent with triple effects of corrosion inhibition, scale inhibition, and wax inhibition. The use of solid slow-release agents greatly simplifies the injection process. Traditional liquid agents require frequent additions, while solid agents can achieve long-term effects through simpler methods (such as one-time injection into the wellbore). Because solid slow-release agents have a long-lasting effect, they can continue to work for a longer period, thus reducing the frequency of agent replacement and injection, thereby reducing agent consumption and overall cost. Solid slow-release agents demonstrate greater adaptability to the problem of difficult injection of liquid agents in some oil wells due to excessive gas content. Solid slow-release agents are not limited by gas content, can exist more stably in the wellbore environment, and can continuously exert their intended effects.

[0023] This invention provides a solid, integrated corrosion inhibitor, scale inhibitor, and wax inhibitor. This three-in-one agent possesses triple functions of corrosion inhibition, scale inhibition, and wax prevention. It has an imidazoline-based structure, a phenyl functional group with wax-inhibiting properties, and a phosphate group with scale-inhibiting effects. The agent is granulated by extrusion to form a solid chemical agent. This three-in-one agent with corrosion inhibition, scale inhibition, and wax prevention is used to suppress corrosion, scaling, and wax formation during oilfield extraction. This functional group-modified three-in-one agent aligns with the current development trend of "one agent with multiple functions" in oilfield chemicals. It can replace existing wellhead injection technology, featuring simple structure, safety and reliability, time and labor saving, long effective period, good energy-saving effect, and high economic benefits, bringing a significant technological breakthrough to oilfield extraction.

[0024] Furthermore, this three-proof agent can be used in a temperature range from room temperature (e.g., 20°C) to 80°C, and can be directly added to the corrosive medium. Attached Figure Description

[0025] Figure 1 This is a diagram of the solid particulate pharmaceutical preparation obtained by the present invention. Detailed Implementation

[0026] To enable those skilled in the art to understand the features and effects of the present invention, the terms and expressions used in the specification and claims are explained and defined in general below. Unless otherwise specified, all technical and scientific terms used herein have the ordinary meaning understood by those skilled in the art regarding the present invention, and in case of conflict, the definitions in this specification shall prevail.

[0027] The theories or mechanisms described and disclosed herein, whether right or wrong, should not in any way limit the scope of the invention, that is, the contents of the invention can be implemented without being limited by any particular theory or mechanism.

[0028] In this document, all features defined by numerical ranges or percentage ranges, such as numerical values, quantities, contents, and concentrations, are for the sake of brevity and convenience only. Accordingly, descriptions of numerical ranges or percentage ranges should be considered as covering and specifically disclosing all possible sub-ranges and individual numerical values ​​(including integers and fractions) within those ranges.

[0029] In this article, unless otherwise specified, “contains,” “includes,” “containing,” “has,” or similar terms cover the meanings of “composed of” and “mainly composed of,” for example, “A contains a” covers the meanings of “A contains a and others” and “A contains only a.”

[0030] For the sake of brevity, not all possible combinations of the technical features in each implementation scheme or embodiment are described herein. Therefore, as long as there is no contradiction in the combination of these technical features, the technical features in each implementation scheme or embodiment can be combined arbitrarily, and all possible combinations should be considered within the scope of this specification.

[0031] This invention provides a solid corrosion inhibitor, scale inhibitor, and wax inhibitor that integrates the preparation method thereof.

[0032] The present invention provides a method for preparing the above-mentioned pharmaceutical agent, the steps of which are as follows:

[0033] S1: Acylation reaction is carried out using polyacrylic acid and hydroxyethyl ethylenediamine as raw materials to generate acylated products; the acylated products are then subjected to cyclization reaction to generate imidazoline compounds; wherein the mass ratio of polyacrylic acid and hydroxyethyl ethylenediamine is (2-4):1;

[0034] S2: The imidazoline product and benzoic acid are subjected to esterification reaction in the presence of a catalyst to obtain an intermediate product; wherein the mass ratio of imidazoline product to benzoic acid is (1~1.2):1; the catalyst is preferably p-toluenesulfonic acid, and the amount of catalyst is 1%;

[0035] S3: The reaction is carried out using epichlorohydrin and sodium phosphate as raw materials to generate a chlorophosphating agent; the mass ratio of epichlorohydrin to sodium phosphate is 1:(1.2~2);

[0036] The intermediate product and the chlorinated phosphating reagent were used as raw materials to carry out a quaternization reaction, with the mass ratio of the intermediate product to the chlorinated phosphating reagent being 1:1; a phosphophenylimidazoline quaternary ammonium salt compound was obtained, and the phosphophenylimidazoline quaternary ammonium salt compound was concentrated to obtain the reagent.

[0037] In S1, the imidazoline compound has corrosion inhibition function, and the imidazoline compound has the following structural formula (I):

[0038]

[0039] The specific steps for S1 are as follows:

[0040] S11: An acylation reaction is carried out using polyacrylic acid and hydroxyethyl ethylenediamine in a mass ratio of (2-4):1 to generate an acylated product. The structural formula of the acylated product is as follows (II):

[0041]

[0042] S12: Take a portion of the acylated product obtained above and perform a cyclization reaction to generate an imidazoline compound;

[0043] The imidazoline compound has the following structural formula (I):

[0044]

[0045] In S11, the mass fraction of the raw material polyacrylic acid is selected as 200-600, and the acylation reaction is carried out at a reaction temperature of 140-170℃ for 6 hours to generate acylated products.

[0046] In step S12, the acylated product is subjected to a cyclization reaction to generate the product compound. This is achieved by subjecting the acylated product to a cyclization reaction at 200-230°C for 4-6 hours, thereby generating the cyclized compound, namely the imidazoline compound.

[0047] S2 yields an intermediate product containing an anti-wax group, which has the following structural formula (III):

[0048]

[0049] S2 provides a strategy for introducing anti-wax groups, the specific steps of which are as follows:

[0050] An imidazoline compound and benzoic acid in a mass ratio of (1-1.2):1 were subjected to an esterification reaction at a temperature of 100-120℃ for 3 hours with p-toluenesulfonic acid as a catalyst to obtain an intermediate product (III) with anti-wax properties.

[0051] S3 yields a phosphophenylimidazoline quaternary ammonium salt compound having the following formula (IV):

[0052]

[0053] S3 provides a strategy for introducing scale-inhibiting functional groups, the specific steps of which are as follows:

[0054] S31: Epichlorohydrin and sodium phosphate in a mass ratio of 1:(1.2~2) are reacted to generate a chlorophosphating agent;

[0055] S32: Using the intermediate product (III) obtained by synthesis and the chlorinated phosphating reagent as raw materials, a quaternization reaction is carried out to obtain the phosphophenylimidazoline quaternary ammonium salt compound (IV).

[0056] S33: A reagent is prepared by concentrating a phosphophenylimidazoline quaternary ammonium salt compound.

[0057] In S31, the synthesis of the chlorophosphating agent involves reacting epichlorohydrin and sodium phosphate at a controlled temperature of 180-200℃ for 2 hours in the presence of the catalyst triphenyl phosphate to obtain the desired chlorophosphating agent.

[0058] In S32, the quaternization reaction involves reacting the intermediate product (III) with a chlorinated phosphating agent at a mass ratio of 1:1 at 85-100℃ for 5 hours with continuous stirring to finally obtain product (IV).

[0059] In S33, the prepared quaternary ammonium salt compound is further concentrated and mixed, and finally molded in one piece by a pressure injection molding machine.

[0060] The specific extrusion granulation parameters are as follows: The start-up load is controlled between 25-30 t / h. During start-up, the load is initially set to 25 t / h. Based on the decreasing current trend, the load is gradually increased. After the start-up valve switches from straight-through to local, the load is increased to approximately 30 t / h. After the start-up valve switches back to straight-through, the load is further increased to 35 t / h. During this period, the main unit current is closely monitored. If the main unit current continues to decrease and approaches the interlock value, the load should be increased promptly. After the above extrusion granulation process, a solid granular agent with corrosion inhibition, scale inhibition, and wax removal properties is finally obtained, such as… Figure 1 As shown.

[0061] The aforementioned phosphophenyl imidazoline quaternary ammonium salt compound is an agent capable of inhibiting corrosion, scaling, and wax formation in wellbores and surface gathering and transportation systems during oilfield development. The imidazoline quaternary ammonium salt compound, prepared through a quaternization reaction, is the key component responsible for its corrosion inhibition effect, while the phosphate and phenyl groups, obtained through a substitution reaction, are crucial for its scale and wax inhibition effects. This three-prevention agent exhibits a highly significant inhibitory effect on metal corrosion, scaling, and wax formation.

[0062] Another aspect of the present invention provides a solid corrosion inhibitor, scale inhibitor, and wax inhibitor prepared by the above-described method, the structural formula of which is as follows:

[0063]

[0064] The above-mentioned agent is a phosphophenylimidazoline quaternary ammonium salt compound with triple effects of corrosion inhibition, scale inhibition, and wax prevention. This compound can be used for corrosion prevention, scale inhibition, and wax prevention in wellbore and surface gathering and transportation systems during oil well production.

[0065] The chemical structure that inhibits corrosion of metal pipelines is mainly composed of imidazoline quaternary ammonium salts, the chemical structure that inhibits scale formation is mainly composed of phosphate groups, and the chemical structure that prevents wax formation is mainly composed of branched benzene rings. This invention, through modification of imidazoline functional groups and improvement of the preparation method of phosphophenylimidazoline quaternary ammonium salt compounds, effectively solves the problem that current conventional agents can only exert a single effect. Through esterification, cyclization, substitution, and other chemical reactions, an agent with triple effects of corrosion inhibition, scale inhibition, and wax prevention is synthesized, which can effectively solve the practical problems of corrosion, scaling, and wax formation in wellbore and surface gathering and transportation systems during current oilfield development.

[0066] Furthermore, through improvements in specific process parameters, and by undergoing processes such as polyemulsification, crushing, mixing, and injection molding, the phosphorophenyl imidazoline quaternary ammonium salt compound with the triple functions of corrosion inhibition, scale inhibition, and wax prevention obtained above is further concentrated into solid particles with a particle size of 5-10 mm.

[0067] The above-mentioned three-proof agents are in line with the current development trend of "one agent with multiple functions" in oilfield chemicals. They can replace the existing wellhead injection technology and have the characteristics of simple structure, safety and reliability, time and labor saving, long effective period, good energy saving effect and high economic benefits.

[0068] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

[0069] The following examples use instruments and equipment conventional in the art. Experimental methods in the following examples, unless otherwise specified, are generally performed under conventional conditions or as recommended by the manufacturer. All raw materials used in the following examples are conventional commercially available products with specifications conventional in the art. In this specification and the following examples, unless otherwise specified, "%" refers to weight percentage, "parts" refers to parts by weight, and "ratio" refers to weight proportion.

[0070] Example 1

[0071] 200g of polyacrylic acid with a molecular weight of 400 and 100g of hydroxyethyl ethylenediamine were added to a three-necked flask. The acylation reaction was carried out at a reaction temperature of 160℃ for 6 hours. After the reaction was completed, the temperature was increased to 220℃ for a cyclization reaction for 5 hours to generate the desired cyclized product, i.e., the imidazoline compound.

[0072] The obtained imidazoline compound (50g) was reacted with 43g of benzoic acid in the presence of the catalyst p-methylbenzenesulfonic acid at a controlled temperature of 100℃ for 3 hours to obtain an intermediate product with anti-wax properties.

[0073] A chlorophosphating agent was prepared by reacting 20g of epichlorohydrin and 24g of sodium phosphate at a controlled temperature of 180℃ for 2 hours in the presence of triphenyl phosphate catalyst.

[0074] 50g of an intermediate product containing anti-wax properties and 50g of chlorinated phosphating reagent were continuously stirred at 90℃ for 5 hours to carry out a quaternization reaction, ultimately obtaining a viscous agent with triple effects of corrosion inhibition, anti-wax, and scale inhibition.

[0075] The viscous agent prepared above is injected into an integrated extrusion granulator. The granulator's start-up load is controlled between 25-30 t / h. During start-up, the load is initially set to 25 t / h. Based on the decreasing current trend, the load is gradually increased. After the start-up valve switches from straight-through to local, the load is increased to approximately 30 t / h. After the start-up valve switches back to straight-through, the load is further increased to 35 t / h. During this period, the main unit current is closely monitored. If the main unit current continues to decrease and approaches the interlock value, the load should be increased promptly. After the above extrusion granulation, a solid granular agent with corrosion inhibition, scale inhibition, and wax removal properties is finally obtained. The specific appearance is as follows. Figure 1 As shown in the figure, the corrosion inhibitor, scale inhibitor, and wax remover combined granular agent prepared in this embodiment has a uniform appearance and a particle size distribution between 5-10 mm.

[0076] Example 2

[0077] 200g of polyacrylic acid with a molecular weight of 400 and 100g of hydroxyethyl ethylenediamine were added to a three-necked flask. The acylation reaction was carried out at a reaction temperature of 160℃ for 6 hours. After the reaction was completed, the temperature was increased to 220℃ for a cyclization reaction for 5 hours to generate the desired cyclized product, i.e., the imidazoline compound.

[0078] The obtained imidazoline compound (50g) was reacted with 46g of benzoic acid in the presence of the catalyst p-toluenesulfonic acid at a temperature of 120℃ for 3 hours to obtain an intermediate product with anti-wax properties.

[0079] A chlorophosphating agent was prepared by reacting 20g of epichlorohydrin and 40g of sodium phosphate at a controlled temperature of 200℃ for 2 hours in the presence of triphenyl phosphate catalyst.

[0080] Mix 50g of an intermediate product containing anti-wax properties with 50g of chlorophosphating agent at 90°C. ℃ The mixture was continuously stirred for 5 hours to carry out a quaternization reaction, ultimately yielding a viscous agent with triple effects of corrosion inhibition, wax inhibition, and scale inhibition. The prepared viscous agent was then injected into an integrated extrusion granulator to prepare a solid granular agent with triple functions of corrosion inhibition, scale inhibition, and wax removal.

[0081] Corrosion inhibition performance evaluation:

[0082] The corrosion inhibition performance was evaluated in accordance with the industry standard SY / T 5273-2000.

[0083] Table 1 shows the comparative evaluation results of the three-proof agent in this embodiment and commercially available oleic acid imidazoline.

[0084] Table 1. Comparative evaluation results of the corrosion inhibitor in this embodiment and commercially available oleic acid imidazoline.

[0085]

[0086] As can be seen from the test data in Table 1, under the same conditions, the corrosion inhibitor prepared in this embodiment has a much better corrosion inhibition performance in corrosive media than commercially available oleic acid imidazoline. At the same time, the three-proof agent prepared in this embodiment can meet the industry requirement that the corrosion rate is not greater than 0.076 mm / a.

[0087] Example 3

[0088] 200g of polyacrylic acid with a molecular weight of 400 and 100g of hydroxyethyl ethylenediamine were added to a three-necked flask. The acylation reaction was carried out at a reaction temperature of 160℃ for 6 hours. After the reaction was completed, the temperature was increased to 220℃ for a cyclization reaction for 5 hours to generate the desired cyclized product, i.e., the imidazoline compound.

[0089] The obtained imidazoline compound (50g) was reacted with 45g of benzoic acid in the presence of the catalyst p-methylbenzenesulfonic acid at a temperature of 120℃ for 3 hours to obtain an intermediate product with anti-wax properties.

[0090] A chlorophosphating agent was prepared by reacting 20g of epichlorohydrin and 30g of sodium phosphate at a temperature of 180℃ for 2 hours in the presence of triphenyl phosphate catalyst.

[0091] 50g of an intermediate product containing anti-wax properties was reacted with 50g of chlorinated phosphating reagent at 90℃ for 5 hours under continuous stirring to carry out a quaternization reaction, ultimately yielding a viscous agent with triple effects of corrosion inhibition, anti-wax, and scale inhibition. The viscous agent prepared above was then injected into an integrated extrusion granulator to prepare a solid granular agent with triple effects of corrosion inhibition, scale inhibition, and wax removal.

[0092] Wax removal performance evaluation:

[0093] Table 2 shows the comparative evaluation results of the corrosion inhibitor and commercially available EVA wax inhibitor in this embodiment.

[0094] Table 2. Comparative evaluation results of the three-proof agent and commercially available EVA wax repellent in this embodiment.

[0095]

[0096] As can be seen from the test data in Table 2, under the same conditions, the three-proof agent prepared in this embodiment has a similar anti-wax effect to that of a specialized anti-wax agent, which can meet the requirements for use in oil fields.

[0097] Example 4

[0098] 200g of polyacrylic acid with a molecular weight of 400 and 100g of hydroxyethyl ethylenediamine were added to a three-necked flask, and an acylation reaction was carried out at 160℃ for 6 hours. After the reaction was completed, the temperature was further increased to 220℃. ℃ The cyclization reaction was carried out for 5 hours to generate the desired cyclization product, namely the imidazoline compound.

[0099] The obtained imidazoline compound (50g) was reacted with 44g of benzoic acid in the presence of the catalyst p-toluenesulfonic acid at a temperature of 115℃ for 3 hours to obtain an intermediate product with anti-wax properties.

[0100] A chlorophosphating reagent was prepared by reacting 20g of epichlorohydrin and 35g of sodium phosphate at a controlled temperature of 200℃ for 2 hours in the presence of triphenyl phosphate catalyst.

[0101] Mix 50g of an intermediate product containing anti-wax properties with 50g of chlorophosphating agent at 90°C.℃ The mixture was continuously stirred for 5 hours to carry out a quaternization reaction, ultimately yielding a viscous agent with triple effects of corrosion inhibition, wax inhibition, and scale inhibition. The prepared viscous agent was then injected into an integrated extrusion granulator to prepare a solid granular agent with triple functions of corrosion inhibition, scale inhibition, and wax removal.

[0102] Scale inhibition performance evaluation:

[0103] Table 3 shows the comparative evaluation results of the corrosion inhibitor and the commercially available HEDP scale inhibitor in this embodiment.

[0104] Table 3. Comparative evaluation results of the corrosion inhibitor and commercially available HEDP scale inhibitor in this embodiment.

[0105]

[0106] As can be seen from the test data in Table 3, under the same conditions, the scale inhibitor prepared in this embodiment has the same scale inhibition performance as the commercially available scale inhibitor HEDP in oilfield formation water, indicating that the scale inhibitor prepared in this embodiment can well meet the scale inhibition requirements in oilfield development.

[0107] Example 5

[0108] 400g of polyacrylic acid with a molecular weight of 200 and 100g of hydroxyethyl ethylenediamine were added to a three-necked flask. The acylation reaction was carried out at a reaction temperature of 140℃ for 6 hours. After the reaction was completed, the temperature was increased to 200℃ for a cyclization reaction for 4 hours to generate the desired cyclized product, i.e., the imidazoline compound.

[0109] The obtained imidazoline compound and 50g of benzoic acid were esterified at 120℃ for 3 hours in the presence of the catalyst p-methylbenzenesulfonic acid to obtain an intermediate product with anti-wax properties.

[0110] A chlorophosphating agent was prepared by reacting 20g of epichlorohydrin and 30g of sodium phosphate at a temperature of 190℃ for 2 hours in the presence of triphenyl phosphate catalyst.

[0111] 50g of an intermediate product containing anti-wax properties was reacted with 50g of a chlorinated phosphating agent at 85°C with continuous stirring for 5 hours to carry out a quaternization reaction, ultimately yielding a viscous agent with triple effects of corrosion inhibition, anti-wax properties, and scale inhibition. The viscous agent prepared above was then injected into an integrated extrusion granulator to prepare a solid granular agent with triple effects of corrosion inhibition, scale inhibition, and wax removal.

[0112] Example 6

[0113] 300g of polyacrylic acid with a molecular weight of 600 and 100g of hydroxyethyl ethylenediamine were added to a three-necked flask. The acylation reaction was carried out at a reaction temperature of 170℃ for 6 hours. After the reaction was completed, the temperature was increased to 230℃ for a cyclization reaction for 6 hours to generate the desired cyclized product, i.e., the imidazoline compound.

[0114] The obtained imidazoline compound (50g) was reacted with 42g of benzoic acid in the presence of the catalyst p-methylbenzenesulfonic acid at a controlled temperature of 100℃ for 3 hours to obtain an intermediate product with anti-wax properties.

[0115] A chlorophosphating agent was prepared by reacting 20g of epichlorohydrin and 40g of sodium phosphate at a controlled temperature of 200℃ for 2 hours in the presence of triphenyl phosphate catalyst.

[0116] 50g of an intermediate product containing anti-wax properties was reacted with 50g of a chlorinated phosphating agent at 100°C with continuous stirring for 5 hours to carry out a quaternization reaction, ultimately yielding a viscous agent with triple effects of corrosion inhibition, anti-wax properties, and scale inhibition. The viscous agent prepared above was then injected into an integrated extrusion granulator to prepare a solid granular agent with triple effects of corrosion inhibition, scale inhibition, and wax removal.

[0117] The above content is only for illustrating the technical concept of the present invention and should not be construed as limiting the scope of protection of the present invention. Any modifications made to the technical solution based on the technical concept proposed in this invention shall fall within the scope of protection of the claims of this invention.

Claims

1. A method for preparing a solid corrosion inhibitor, scale inhibitor, and wax inhibitor that integrates the functions of corrosion inhibition, scale inhibition, and wax prevention, characterized in that, Includes the following steps: S1: Acylation reaction is carried out using polyacrylic acid and hydroxyethyl ethylenediamine as raw materials to generate acylated products; The acylation product was subjected to a cyclization reaction to generate an imidazoline compound; S2: An intermediate product is obtained by esterification of imidazoline compound and benzoic acid in the presence of a catalyst. S3: Epichlorohydrin and sodium phosphate are reacted to generate a chlorinated phosphating agent; the intermediate product and the chlorinated phosphating agent are used as raw materials to carry out a quaternization reaction to obtain a phosphophenylimidazoline quaternary ammonium salt compound; the phosphophenylimidazoline quaternary ammonium salt compound is concentrated to obtain the reagent.

2. The preparation method of the solid corrosion inhibitor, scale inhibitor, and wax inhibitor integrated agent according to claim 1, characterized in that, In S1, the mass ratio of polyacrylic acid and hydroxyethyl ethylenediamine is (2~4):

1.

3. The preparation method of the solid corrosion inhibitor, scale inhibitor, and wax inhibitor integrated agent according to claim 1, characterized in that, In S1, the molecular weight of the polyacrylic acid is selected to be 200-600; the reaction temperature of the acylation reaction is 140-170℃, and the reaction time of the acylation reaction is 6h; the reaction temperature of the cyclization reaction is 200-230℃, and the reaction time of the cyclization reaction is 4-6h.

4. The preparation method of the solid corrosion inhibitor, scale inhibitor, and wax inhibitor integrated agent according to claim 1, characterized in that, In S2, the mass ratio of the imidazoline compound to benzoic acid is (1~1.2):

1.

5. The preparation method of the solid corrosion inhibitor, scale inhibitor, and wax inhibitor integrated agent according to claim 1, characterized in that, In S2, the catalyst is p-toluenesulfonic acid; The esterification reaction is carried out at a temperature of 100-120 °C for 3 hours.

6. The preparation method of the solid corrosion inhibitor, scale inhibitor, and wax inhibitor integrated agent according to claim 1, characterized in that, In S3, the mass ratio of epichlorohydrin to sodium phosphate is 1:(1.2~2).

7. The preparation method of the solid corrosion inhibitor, scale inhibitor, and wax inhibitor as described in claim 1 or 6, characterized in that, In step S3, the preparation method of the chlorinated phosphorylating agent is as follows: A chlorophosphating agent was prepared by reacting epichlorohydrin and sodium phosphate in the presence of triphenyl phosphate catalyst at a controlled temperature of 180-200 °C for 2 hours.

8. The preparation method of the solid corrosion inhibitor, scale inhibitor, and wax inhibitor integrated agent according to claim 1, characterized in that, In step S3, the mass ratio of the intermediate product to the chlorinated phosphating agent is 1:

1. The quaternization reaction is carried out at a temperature of 85-100 °C for 5 hours.

9. The preparation method of the integrated solid corrosion inhibitor, scale inhibitor, and wax inhibitor according to claim 1, characterized in that, In step S3, the process of concentrating the agent to obtain the medicine is as follows: The phosphophenylimidazoline quaternary ammonium salt compound was concentrated and mixed, and then integrally molded by pressure injection molding to obtain the drug.

10. A solid corrosion inhibitor, scale inhibitor, and wax inhibitor prepared by the method for preparing a solid corrosion inhibitor, scale inhibitor, and wax inhibitor according to any one of claims 1 to 9.

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