CN111020597B - Oil-soluble corrosion inhibitor for gas well oil pipe and preparation method thereof - Google Patents

Oil-soluble corrosion inhibitor for gas well oil pipe and preparation method thereof Download PDF

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CN111020597B
CN111020597B CN201911339828.9A CN201911339828A CN111020597B CN 111020597 B CN111020597 B CN 111020597B CN 201911339828 A CN201911339828 A CN 201911339828A CN 111020597 B CN111020597 B CN 111020597B
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oil
corrosion inhibitor
gas well
imidazoline
soluble corrosion
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CN111020597A (en
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张磊
贺华镭
苟利鹏
杨金峰
张进科
陈岑
李欢
吴阳
李乐
徐磊
丁平平
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Xi'an Sanwei Technology Development Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
    • C23F11/14—Nitrogen-containing compounds
    • C23F11/149—Heterocyclic compounds containing nitrogen as hetero atom
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/54—Compositions for in situ inhibition of corrosion in boreholes or wells
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/32—Anticorrosion additives

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Abstract

The invention discloses an oil soluble corrosion inhibitor for gas well oil pipe and a preparation method thereof,the corrosion inhibitor is used for solving the problem that the stability and the corrosion prevention effect of the corrosion inhibitor are influenced by imidazoline ring opening caused by long-term storage of the prior imidazoline corrosion inhibitor. According to the mass fraction, the raw materials of the corrosion inhibitor comprise 20-30% of a main agent and 70-80% of a compound, wherein the main agent is imidazoline Schiff base, and the compound comprises 10-15% of aromatic azole, 5-10% of hydroxyethyl sulphosuccinic acid and 45-65% of a solvent based on the total mass of the oil soluble corrosion inhibitor for the oil well tubing. The corrosion inhibitor obtained by the invention is suitable for a gas well oil pipe with low water content, can be quickly adsorbed on the inner wall of the pipe, can be adsorbed in the gas well oil pipe to form a layer of compact corrosion inhibitor protective film for CO-containing gas2Carbon steel pipelines and equipment in the gas well environment of gas have good protection effect. Has the characteristics of good plane spreadability and good compatibility of diesel oil, crude oil, condensate oil and the like.

Description

Oil-soluble corrosion inhibitor for gas well oil pipe and preparation method thereof
Technical Field
The invention relates to the technical field of gas well oil pipe and equipment protection in the petroleum and petrochemical field, in particular to an oil-soluble corrosion inhibitor for a gas well oil pipe and a preparation method thereof.
Background
Effectively controls the corrosion in the sulfur-containing environment, and is an economic and effective measure by applying the corrosion inhibitor technology while reasonably selecting materials. The use of the corrosion inhibitor is an important method for corrosion prevention at home and abroad, and the specific corrosion inhibition treatment process is determined according to the characteristics of the gathering and transportation system.
At present, industrial corrosion inhibitors used at home and abroad are basically adsorption type corrosion inhibitors, such as Mannich bases, imidazoline derivatives, pyridine, quinoline quaternary ammonium salts, alkynols, high molecular polymers and the like. The general adsorption type corrosion inhibitor is characterized in that the corrosion inhibitor can be stably adsorbed on the surface of metal to form a compact corrosion inhibitor protective film, thereby effectively preventing a corrosive medium from diffusing and permeating to the surface of the metal to achieve the purpose of retarding or inhibiting corrosion. The corrosion inhibitor commonly used in oilfield pipeline systems mainly comprises imidazoline and derivatives thereof, polyol phosphate and the like. Wherein the imidazoline and the derivatives thereof are used in the largest amount due to the advantages of small dosage, excellent corrosion inhibition performance and the like.
A corrosion inhibitor developed in the patent of Duffo Chaoyang, its preparation method (CN201010158037.9), and an anti-H agent2S/CO2The corrosion inhibitor under combined action (CN1966774) and a water-soluble imidazoline amide corrosion inhibitor and the preparation and use methods (CN101705112A) thereof are imidazoline corrosion inhibitors, but the corrosion inhibitor can cause imidazoline ring opening after being stored for a long time, thereby influencing the stability and the corrosion prevention effect of the corrosion inhibitor.
Disclosure of Invention
The invention provides an oil soluble corrosion inhibitor for a gas well oil pipe and a preparation method thereof, which are used for solving the problem that the stability and the corrosion prevention effect of the corrosion inhibitor are influenced by imidazoline ring opening caused by long-term storage of the existing imidazoline corrosion inhibitor.
The technical solution of the invention is as follows: an oil soluble corrosion inhibitor for gas well oil pipes comprises, by mass, 20-30% of a main agent and 70-80% of a compound, wherein the main agent is imidazoline Schiff base, and the structural formula of the imidazoline Schiff base is as follows:
Figure GDA0003301393100000021
wherein n is less than or equal to 3,
the compound is composed of 10-15% of aromatic azole, 5-10% of hydroxyethyl thiosuccinic acid and 45-65% of solvent by total mass of the oil soluble corrosion inhibitor for the oil well oil pipe.
The main agent is a product synthesized according to the following steps:
adding aspartic acid and polyethylene polyamine amine into a reaction kettle according to the mol ratio of 1:1.2-1.5, adding water-carrying agent xylene which is 10-12% of the total amount of the amine and the acid, heating and stirring to 150 ℃ and 160 ℃, preserving heat for 3-4 hours, wherein the heating speed is not higher than 20 ℃/10min, water flows out from a condensation pipe at the top of the reaction kettle in the reaction process, the generated amide is continuously heated to 170 ℃ and 180 ℃, and reacting for 1.5-2 hours; continuously heating at a heating speed of not higher than 20 ℃/10min, preserving heat for 3-4h at the temperature of 210-220 ℃, cooling to below 50 ℃, sampling and testing the acid value, and obtaining an imidazoline intermediate when the acid value is less than 5 mg/kg;
then mixing imidazoline and aromatic aldehyde in isopropanol with the molar ratio of 1:1.2-1.4 accounting for 50-60% of the total amount of the imidazoline and the aromatic aldehyde uniformly, and heating to 70-80 ℃ of the isopropanol to obtain the imidazoline Schiff base;
the reaction formula is as follows:
the first step is as follows: amidation reaction
Figure GDA0003301393100000022
The second step is that: cyclization reaction
Figure GDA0003301393100000023
The third step: schiff base reaction
Figure GDA0003301393100000031
The polyethylene polyamine amine is one of diethylenetriamine and tetraethylenepentamine.
The aromatic aldehyde is cinnamaldehyde.
The reflux temperature of the isopropanol is 70-80 DEG C
The aromatic azole in the compound is selected from benzotriazole, methylbenzotriazole and mercaptobenzothiazole.
The solvent in the compound is selected from one of solvent naphtha 100#, solvent naphtha 200# and diesel oil.
A preparation method of an oil soluble corrosion inhibitor for an oil pipe of a gas well comprises the following steps:
(1) mixing and uniformly stirring 10-15% of aromatic azole, 5-10% of hydroxyethyl thiosuccinic acid and 45-65% of solvent by the total mass of the oil soluble corrosion inhibitor for the oil pipe of the gas well to obtain a compound;
(2) according to the mass fraction, 20-30% of the main agent and 70-80% of the compound are mixed and stirred evenly to obtain the finished product.
The invention provides an oil-soluble corrosion inhibitor for an oil pipe of a gas well and a preparation method thereof, the corrosion inhibitor can be widely applied to an oil-gas field and gas well system, corrosion prevention evaluation is carried out on the corrosion inhibitor according to the content of the industrial standard SY/T5273-2014 corrosion inhibitor performance index and evaluation method for water treatment produced in the oil field, corrosion perforation in an air pipeline can be effectively controlled, the corrosion inhibitor is suitable for the oil pipe of the gas well with low water content, can be quickly adsorbed on the inner wall of the pipeline, can be adsorbed in the oil pipe of the gas well to form a layer of compact corrosion inhibitor protective film, and can be used for adsorbing a CO-containing protective film of the corrosion inhibitor in the oil pipe of the gas well2The carbon steel pipeline and equipment in the gas pipeline environment have good protection effect. After the Schiff base is introduced, the surface spreadability on the metal surface is better, and the imidazoline ring is less prone to desorption. The synthesis of imidazoline Schiff base increases the film forming firmness of corrosion inhibitor molecules on the inner wall of the pipeline, and has the characteristics of good plane spreadability and good compatibility of diesel oil, crude oil, condensate oil and the like in an oil-gas field gas pipeline.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making creative efforts, based on the embodiments of the present invention, belong to the scope of protection of the present invention, and in the context of the present invention the terms "oil well drilling, production and storage system" and "gas well drilling, production and storage system" comprise all corrosion-prone pipes and equipment for drilling, producing and storing oil and gas from underground formations.
Example 1
The embodiment 1 of the invention provides an oil-soluble corrosion inhibitor for an oil pipe of a gas well, which comprises, by mass, 25% of a main agent and 75% of a compound, wherein the main agent is imidazoline Schiff base, and the compound comprises, based on the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well, 10% of benzotriazole, 7% of hydroxyethyl thiosuccinic acid and 58% of solvent oil 200 #.
Specifically, the preparation method of the oil soluble corrosion inhibitor for the gas well oil pipe comprises the following steps:
(1) adding aspartic acid and diethylenetriamine into a reaction kettle according to a molar ratio of 1:1.2 for reaction, and simultaneously adding xylene as a water carrying agent, wherein the xylene carrying agent is 10% of the total mass of an oil soluble corrosion inhibitor for an oil well oil pipe, heating, stirring, raising the temperature to 150-;
uniformly mixing the obtained imidazoline intermediate and cinnamon oil in isopropanol (accounting for 50% of the total amount of the imidazoline and the cinnamon oil), heating to the isopropanol reflux temperature of 70-80 ℃ to obtain a main agent imidazoline Schiff base, wherein the molar ratio of the imidazoline intermediate to the cinnamon oil is 1: 1.4;
the reaction formula is as follows:
the first step is as follows: amidation reaction
Figure GDA0003301393100000041
The second step is that: cyclization reaction
Figure GDA0003301393100000051
The third step: schiff base reaction
Figure GDA0003301393100000052
(2) Mixing and stirring 10% of benzotriazole, 7% of hydroxyethyl thiosuccinic acid and 58% of solvent oil 200# uniformly based on the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well to obtain a compound;
(3) and (3) mixing and uniformly stirring 25% of the main agent obtained in the step (1) and 75% of the compound obtained in the step (2) according to the mass fraction to obtain a finished product, namely code SW-01.
Example 2
The embodiment 2 of the invention provides an oil-soluble corrosion inhibitor for an oil pipe of a gas well, which comprises the following raw materials of, by mass, 20% of a main agent and 80% of a compound, wherein the main agent is imidazoline Schiff base, the compound is composed of, by mass, 15% of aromatic azole, 10% of hydroxyethyl thiosuccinic acid and 55% of a solvent, based on the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well.
Wherein, the aromatic azole is mercaptobenzothiazole, and the solvent is mineral spirit 100 #.
Specifically, the preparation method of the oil soluble corrosion inhibitor for the gas well oil pipe comprises the following steps:
(1) adding aspartic acid and triethylene tetramine into a reaction kettle according to a molar ratio of 1:1.5 for reaction, and simultaneously adding a xylene water carrying agent, wherein the xylene water carrying agent is 10% of the total mass of an oil soluble corrosion inhibitor for an oil well oil pipe, heating, stirring, raising the temperature to 150 ℃ and 160 ℃, preserving heat for 3h, wherein the heating rate is less than or equal to 20 ℃/10min, water flows out of a condensation pipe at the top of the reaction kettle in the reaction process, the generated amide is then heated to 170 ℃ and 180 ℃ for reaction for 1.5h, then heating to 210 ℃, preserving heat for 4h at 210 ℃ and 220 ℃, wherein the heating rate is less than or equal to 20 ℃/10min, then cooling to below 50 ℃, sampling and testing the acid value, and the acid value is less than 5mg/kg, thus obtaining an imidazoline intermediate;
uniformly mixing the obtained imidazoline intermediate and cinnamon oil in isopropanol (accounting for 50% of the total amount of the imidazoline and the cinnamon oil), heating to 70-80 ℃ to obtain a main agent imidazoline Schiff base, wherein the molar ratio of the imidazoline intermediate to the cinnamon oil is 1: 1.2;
the reaction formula is as follows:
the first step is as follows: amidation reaction
Figure GDA0003301393100000061
The second step is that: cyclization reaction
Figure GDA0003301393100000062
The third step: schiff base reaction
Figure GDA0003301393100000063
(2) Mixing and stirring 15% of mercaptobenzothiazole, 10% of hydroxyethyl thiosuccinic acid and 55% of solvent oil 100# uniformly by the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well to obtain a compound;
(3) and (3) mixing and uniformly stirring 20% of the main agent obtained in the step (1) and 80% of the compound obtained in the step (2) according to the mass fraction to obtain a finished product, namely code SW-02.
Example 3
The embodiment 3 of the invention provides an oil-soluble corrosion inhibitor for an oil pipe of a gas well, which comprises the following raw materials of, by mass, 20% of a main agent and 80% of a compound, wherein the main agent is imidazoline Schiff base, the compound is composed of, by mass, 10% of aromatic azole, 5% of hydroxyethyl thiosuccinic acid and 65% of a solvent, based on the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well.
Wherein, the aromatic azole is methylbenzotriazole, and the solvent is mineral spirit 100 #.
Specifically, the preparation method of the oil soluble corrosion inhibitor for the gas well oil pipe comprises the following steps:
(1) adding aspartic acid and tetraethylenepentamine into a reaction kettle according to a molar ratio of 1:1.5 for reaction, and simultaneously adding a xylene water carrying agent, wherein the xylene water carrying agent is 10% of the total mass of an oil soluble corrosion inhibitor for an oil well oil pipe, heating, stirring, raising the temperature to 150-;
uniformly mixing the obtained imidazoline intermediate and cinnamon oil in isopropanol (accounting for 50% of the total amount of the imidazoline and the cinnamon oil), heating to 70-80 ℃ to obtain a main agent imidazoline Schiff base, wherein the molar ratio of the imidazoline intermediate to the cinnamon oil is 1: 1.4;
the reaction formula is as follows:
the first step is as follows: amidation reaction
Figure GDA0003301393100000071
The second step is that: cyclization reaction
Figure GDA0003301393100000072
The third step: schiff base reaction
Figure GDA0003301393100000073
(2) Mixing and stirring 10% of methylbenzotriazole, 5% of hydroxyethyl thiosuccinic acid and 65% of solvent oil 100# uniformly by the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well to obtain a compound;
(3) and (3) mixing and uniformly stirring 20% of the main agent obtained in the step (1) and 80% of the compound obtained in the step (2) according to the mass fraction to obtain a finished product, namely code SW-03.
Example 4
The embodiment 4 of the invention provides an oil-soluble corrosion inhibitor for an oil pipe of a gas well, which comprises, by mass, 30% of a main agent and 70% of a compound, wherein the main agent is imidazoline Schiff base, and the compound comprises, by mass of the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well, 10% of aromatic azole, 10% of hydroxyethyl thiosuccinic acid and 50% of a solvent.
Wherein, the aromatic azole is methylbenzotriazole, and the solvent is diesel oil.
Specifically, the preparation method of the oil soluble corrosion inhibitor for the gas well oil pipe comprises the following steps:
(1) adding aspartic acid and tetraethylenepentamine into a reaction kettle according to a molar ratio of 1:1.2 for reaction, and simultaneously adding a xylene water carrying agent, wherein the xylene water carrying agent is 10% of the total mass of an oil soluble corrosion inhibitor for an oil well oil pipe, heating, stirring and heating to 150-;
uniformly mixing the obtained imidazoline intermediate and cinnamon oil in isopropanol (accounting for 50% of the total amount of the imidazoline and the cinnamon oil), heating to 70-80 ℃ to obtain a main agent imidazoline Schiff base, wherein the molar ratio of the imidazoline intermediate to the cinnamon oil is 1: 1.4;
the reaction formula is as follows:
the first step is as follows: amidation reaction
Figure GDA0003301393100000081
The second step is that: cyclization reaction
Figure GDA0003301393100000091
The third step: schiff base reaction
Figure GDA0003301393100000092
(2) Mixing and stirring evenly 10% of methylbenzotriazole, 10% of hydroxyethyl thiosuccinic acid and 50% of diesel oil by the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well to obtain a compound;
(3) and (3) mixing and uniformly stirring 30% of the main agent obtained in the step (1) and 70% of the compound obtained in the step (2) according to the mass fraction to obtain a finished product, namely code SW-04.
Example 5
The embodiment 5 of the invention provides an oil-soluble corrosion inhibitor for an oil pipe of a gas well, which comprises the following raw materials of, by mass, 20% of a main agent and 80% of a compound, wherein the main agent is imidazoline Schiff base, the compound is composed of, by mass, 15% of aromatic azole, 10% of hydroxyethyl thiosuccinic acid and 55% of a solvent, based on the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well.
Wherein, the aromatic azole is benzotriazole, and the solvent is mineral spirit 100 #.
Specifically, the preparation method of the oil soluble corrosion inhibitor for the gas well oil pipe comprises the following steps:
(1) adding aspartic acid and diethylenetriamine into a reaction kettle for reaction according to the molar ratio of 1:1.5, and simultaneously adding a xylene water carrying agent, wherein the xylene water carrying agent is 10% of the total mass of the oil-soluble corrosion inhibitor for the oil-well oil pipe, heating, stirring and heating to 150-;
uniformly mixing the obtained imidazoline intermediate and cinnamaldehyde in isopropanol (accounting for 50% of the total amount of the imidazoline and the cinnamaldehyde), heating to 70-80 ℃ to obtain a main agent imidazoline Schiff base, wherein the molar ratio of the imidazoline intermediate to the cinnamaldehyde is 1: 1.4;
the reaction formula is as follows:
the first step is as follows: amidation reaction
Figure GDA0003301393100000101
The second step is that: cyclization reaction
Figure GDA0003301393100000102
The third step: schiff base reaction
Figure GDA0003301393100000103
(2) Mixing and stirring uniformly 15% of benzotriazole, 10% of hydroxyethyl thiosuccinic acid and 55% of solvent oil 100# by the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well to obtain a compound;
(3) and (3) mixing and uniformly stirring 20% of the main agent obtained in the step (1) and 80% of the compound obtained in the step (2) according to the mass fraction to obtain a finished product, namely code SW-05.
Example 6
The embodiment 6 of the invention provides an oil-soluble corrosion inhibitor for an oil pipe of a gas well, which comprises the following raw materials of, by mass, 25% of a main agent and 75% of a compound, wherein the main agent is imidazoline Schiff base, the compound is calculated by the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well, and the compound is composed of 15% of aromatic azole, 6% of hydroxyethyl thiosuccinic acid and 54% of a solvent.
Wherein, the aromatic azole is mercaptobenzothiazole, and the solvent is diesel oil.
Specifically, the preparation method of the oil soluble corrosion inhibitor for the gas well oil pipe comprises the following steps:
(1) adding aspartic acid and tetraethylenepentamine into a reaction kettle according to a molar ratio of 1:1.5 for reaction, and simultaneously adding a xylene water carrying agent, wherein the xylene water carrying agent is 10% of the total mass of an oil soluble corrosion inhibitor for an oil well oil pipe, heating, stirring, raising the temperature to 150-;
uniformly mixing the obtained imidazoline intermediate and cinnamaldehyde in isopropanol (accounting for 50% of the total amount of imidazoline and cinnamon oil), heating to 70-80 ℃ to obtain a main agent imidazoline Schiff base, wherein the molar ratio of the imidazoline intermediate to the cinnamon oil is 1: 1.4;
the reaction formula is as follows:
the first step is as follows: amidation reaction
Figure GDA0003301393100000111
The second step is that: cyclization reaction
Figure GDA0003301393100000112
The third step: schiff base reaction
Figure GDA0003301393100000113
(2) Mixing and uniformly stirring 15% of sulfenyl benzothiazole, 6% of hydroxyethyl thiosuccinic acid and 54% of diesel oil by the total mass of the oil soluble corrosion inhibitor for the oil pipe of the gas well to obtain a compound;
(3) and (3) mixing and uniformly stirring 25% of the main agent obtained in the step (1) and 75% of the compound obtained in the step (2) according to the mass fraction to obtain a finished product, namely code SW-06.
Example 7
The embodiment 7 of the invention provides an oil-soluble corrosion inhibitor for an oil pipe of a gas well, which comprises 28 mass percent of main agent and 72 mass percent of compound according to mass fraction, wherein the main agent is imidazoline Schiff base, the compound is calculated by the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well, and the compound is composed of 10 mass percent of aromatic azole, 5 mass percent of hydroxyethyl thiosuccinic acid and 57 mass percent of solvent.
Wherein, the aromatic azole is benzotriazole, and the solvent is mineral spirit 200 #.
Specifically, the preparation method of the oil soluble corrosion inhibitor for the gas well oil pipe comprises the following steps:
(1) adding aspartic acid and diethylenetriamine into a reaction kettle for reaction according to the molar ratio of 1:1.5, and simultaneously adding a xylene water carrying agent, wherein the xylene water carrying agent is 10% of the total mass of the oil-soluble corrosion inhibitor for the oil-well oil pipe, heating, stirring and heating to 150-;
uniformly mixing the obtained imidazoline intermediate and benzaldehyde in isopropanol (accounting for 50% of the total amount of imidazoline and cinnamon oil), heating to 70-80 ℃ to obtain a main agent imidazoline Schiff base, wherein the molar ratio of the imidazoline intermediate to the benzaldehyde is 1: 1.2;
the reaction formula is as follows:
the first step is as follows: amidation reaction
Figure GDA0003301393100000121
The second step is that: cyclization reaction
Figure GDA0003301393100000122
The third step: schiff base reaction
Figure GDA0003301393100000123
(2) Mixing and stirring 10% of benzotriazole, 5% of hydroxyethyl thiosuccinic acid and 57% of solvent oil 200# uniformly based on the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well to obtain a compound;
(3) and (3) mixing and uniformly stirring 28% of the main agent obtained in the step (1) and 72% of the compound obtained in the step (2) according to the mass fraction to obtain a finished product, namely code SW-07.
Example 8
The embodiment 8 of the invention provides an oil-soluble corrosion inhibitor for an oil pipe of a gas well, which comprises the following raw materials of, by mass, 20% of a main agent and 80% of a compound, wherein the main agent is imidazoline Schiff base, the compound is composed of 12% of aromatic azole, 6% of hydroxyethyl thiosuccinic acid and 62% of a solvent, based on the total mass of the oil-soluble corrosion inhibitor for the oil pipe of the gas well.
Wherein, the aromatic azole is mercaptobenzothiazole, and the solvent is diesel oil.
Specifically, the preparation method of the oil soluble corrosion inhibitor for the gas well oil pipe comprises the following steps:
(1) adding aspartic acid and polyethylene polyamine into a reaction kettle according to a molar ratio of 1:1.5 for reaction, and simultaneously adding a xylene water carrying agent, wherein the xylene water carrying agent is 10% of the total mass of the oil soluble corrosion inhibitor for the oil well oil pipe, heating, stirring and heating to 150-;
uniformly mixing the obtained imidazoline intermediate and cinnamaldehyde in isopropanol (accounting for 50% of the total amount of imidazoline and cinnamon oil), heating to 70-80 ℃ to obtain a main agent imidazoline Schiff base, wherein the molar ratio of the imidazoline intermediate to the cinnamaldehyde is 1: 1.4;
the reaction formula is as follows:
the first step is as follows: amidation reaction
Figure GDA0003301393100000131
The second step is that: cyclization reaction
Figure GDA0003301393100000132
The third step: schiff base reaction
Figure GDA0003301393100000141
(2) Mixing and stirring 12% of mercaptobenzothiazole, 6% of hydroxyethyl thiosuccinic acid and 62% of diesel oil uniformly based on the total mass of the oil soluble corrosion inhibitor for the oil pipe of the gas well to obtain a compound;
(3) and (3) mixing and uniformly stirring 20% of the main agent obtained in the step (1) and 80% of the compound obtained in the step (2) according to the mass fraction to obtain a finished product, namely code SW-08.
Example 9
In order to test the protection effect of the corrosion inhibitor on the gathering and transportation pipeline, a high-temperature and high-pressure experimental system is adopted to simulate the environment of a gas well system, simulated water is prepared, and the corrosion inhibition effect of the oil-soluble corrosion inhibitor for the gas well oil pipe in the embodiments 1-8 is evaluated according to the corrosion index specification (the corrosion inhibition rate is more than or equal to 70%) in the standard of SY/T5273-2014 corrosion inhibitor performance index and evaluation method for oilfield produced water treatment in the industry standard.
The experimental conditions used in the simulation are shown in table 1, the chemical reagent dosage for preparing 3L of simulation water is shown in table 2, and the material of the hanging piece sample is N80.
TABLE 1 evaluation parameters of the simulation test
Item Test conditions
Temperature, C 70
Total pressure, MPa 20
CO2Partial pressure, MPa 1.2
Test time, day 3
TABLE 2 preparation of chemical reagent dosage for 3L of simulated water
Figure GDA0003301393100000142
Figure GDA0003301393100000151
Through high-temperature and high-pressure tests, working condition environments in the tables 1 and 2 are simulated, and test results are shown in the table 3 under the condition that the test period is 7 days.
TABLE 3 Corrosion inhibitor Corrosion evaluation results
Figure GDA0003301393100000152
As can be seen from Table 3, in examples 1-8, the oil-soluble corrosion inhibitors for the oil well tubing have corrosion inhibition rates of more than 90%, meet the corrosion index specification of the standard SY/T5273-2014 (the corrosion inhibition rate is more than or equal to 70%), and have excellent corrosion prevention effects.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.

Claims (7)

1. An oil-soluble corrosion inhibitor for gas well oil pipes is characterized in that the oil-soluble corrosion inhibitor comprises, by mass, 20-30% of a main agent and 70-80% of a compound, wherein the main agent is imidazoline Schiff base, and the structural formula of the imidazoline Schiff base is as follows:
Figure FDA0003304807750000011
wherein n is less than or equal to 3;
the compound is composed of 10-15% of aromatic azole, 5-10% of hydroxyethyl thiosuccinic acid and 45-65% of solvent by the total mass of the oil soluble corrosion inhibitor for the oil well oil pipe;
the main agent is a product synthesized according to the following steps:
adding aspartic acid and polyethylene polyamine amine into a reaction kettle according to the mol ratio of 1:1.2-1.5, adding water-carrying agent xylene which is 10-12% of the total material amount of the acid and the amine, heating and stirring to 150 ℃ and 160 ℃, preserving heat for 3-4 hours, wherein the heating speed is not higher than 20 ℃/10min, water flows out from a condensation pipe at the top of the reaction kettle in the reaction process, the generated amide is generated, continuously heating to 170 ℃ and 180 ℃, and reacting for 1.5-2 hours; continuously heating at a heating speed of not higher than 20 ℃/10min, preserving heat for 3-4h at the temperature of 210-220 ℃, cooling to below 50 ℃, sampling and testing the acid value, and obtaining an imidazoline intermediate when the acid value is less than 5 mg/kg;
then evenly mixing imidazoline and aromatic aldehyde in isopropanol which accounts for 50-60% of the total amount of the imidazoline and the aromatic aldehyde according to the molar ratio of 1:1.2-1.4, and heating to the reflux temperature of the isopropanol to obtain the imidazoline Schiff base;
the reaction formula is as follows:
the first step is as follows: amidation reaction
Figure FDA0003304807750000021
The second step is that: cyclization reaction
Figure FDA0003304807750000022
The third step: schiff base reaction
Figure FDA0003304807750000023
。
2. The oil soluble corrosion inhibitor for gas well oil pipes as claimed in claim 1, wherein the polyethylene polyamine is selected from one of diethylenetriamine and tetraethylenepentamine.
3. The oil soluble corrosion inhibitor for gas well tubing of claim 1 wherein the aromatic aldehyde is cinnamaldehyde.
4. The method of preparing an oil soluble corrosion inhibitor for gas well tubing of claim 1 wherein the reflux temperature of the isopropyl alcohol is 70-80 ℃.
5. The oil soluble corrosion inhibitor for gas well oil pipes as claimed in claim 1, wherein the aromatic azole in the compound is one of benzotriazole, tolyltriazole and mercaptobenzothiazole.
6. The oil-soluble corrosion inhibitor for gas well oil pipes as claimed in claim 1, wherein the solvent in the compound is selected from one of mineral spirit 100#, mineral spirit 200#, and diesel oil.
7. A method of preparing an oil soluble corrosion inhibitor for gas well tubing as claimed in any one of claims 1 to 6 comprising the steps of:
(1) mixing and uniformly stirring 10-15% of aromatic azole, 5-10% of hydroxyethyl thiosuccinic acid and 45-65% of solvent by the total mass of the oil soluble corrosion inhibitor for the oil pipe of the gas well to obtain a compound;
(2) according to the mass fraction, 20-30% of the main agent and 70-80% of the compound are mixed and stirred evenly to obtain the finished product.
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