CN111719158A - Corrosion inhibitor composition suitable for wide flow rate range and preparation method thereof - Google Patents

Corrosion inhibitor composition suitable for wide flow rate range and preparation method thereof Download PDF

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CN111719158A
CN111719158A CN202010458259.6A CN202010458259A CN111719158A CN 111719158 A CN111719158 A CN 111719158A CN 202010458259 A CN202010458259 A CN 202010458259A CN 111719158 A CN111719158 A CN 111719158A
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corrosion inhibitor
inhibitor composition
component
formula
acid
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CN111719158B (en
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赵晴晴
付德利
孟庆东
孙征宇
王冬彬
孙琳琳
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Dongying Dongfang Chemical Industrial Co ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-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
    • C23F11/00Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • C23F11/08Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
    • C23F11/10Inhibiting 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

Abstract

The invention relates to a corrosion inhibitor composition suitable for a wide flow rate range and a manufacturing method thereof, wherein the corrosion inhibitor composition comprises the following components: about 100 to 200 parts by weight of an imidazoline-based component, about 30 to 100 parts by weight of an amidothiourea component, and optionally, the corrosion inhibitor composition may further include 1 to 20 parts by weight of an auxiliary component. According to the scheme of the invention, the composition has good corrosion prevention effect in a high-speed flowing corrosive liquid environment or a low-speed slow-flowing corrosive liquid environment.

Description

Corrosion inhibitor composition suitable for wide flow rate range and preparation method thereof
Technical Field
The invention relates to the field of organic chemistry and petrochemical industry, in particular to a corrosion inhibitor composition, and more particularly relates to a corrosion inhibitor composition suitable for produced water of an oil field, especially suitable for the produced water in a wide flow velocity range.
Background
China is a country with large energy demand and consumption in the world, and energy such as petroleum and the like related to national safety is of great importance to the operation development of industrial enterprises and the smooth operation of society. The petroleum storage in China is seriously heterogeneous, and the petroleum storage is usually mined in a water injection mode, so that a large amount of injected water and produced water are required to be used in the mining process, and the water circulation is realized. The production and circulation of water injection causes soaking and corrosion of the circulating equipment, such as pipelines and circulating water equipment, and particularly under conditions of high pressure and different fluidity, metal corrosion phenomena of different mechanisms and degrees can occur. Therefore, there is a need to use appropriate corrosion inhibitors for produced water from water flooding fields to prevent damage to equipment, particularly metals, from high temperature and high pressure flowing water.
Many scholars and engineers have made experiments and contributions to the study of corrosion inhibitors. Researches show that the corrosion prevention effect of the corrosion inhibitor is related to the flowing speed of fluid, some corrosion inhibitors or corrosion inhibitors have good corrosion inhibition effect when the fluid is higher than a certain minimum critical strength, and the protective film formed by the corrosion inhibitor is damaged under the conditions of shear stress and the like in the environment with very high fluid speed. It is often desirable to use different types of corrosion protection or inhibitor components for different fluid rates and application environments, which presents new challenges for field mining applications.
For example, Chinese patent CN103849879B discloses a bimolecular Schiff base sewage corrosion inhibitor and a preparation method thereof, wherein the corrosion inhibitor component of the method contains bimolecular Schiff base compound 1, 5-bis (hydroxyphenylhydrazinyl) -pentane, and the invention considers that the factors of small addition amount, high production efficiency and the like are obtained. However, in practice, the double-center corrosion inhibitor component of similar cyclic or chain macromolecules has a good effect in an application environment with a high fluid speed, but the corrosion resistance is not good enough in the field of long-term soaking type produced water corrosion resistance with a low fluid speed. Similar inventions have not recognized the effect of produced water flow velocity on corrosion protection.
Therefore, there is a need in the art for a corrosion protection liquid that can be used in high temperature and corrosive produced water, and that can achieve good corrosion protection in a high flow rate corrosive liquid environment or a low flow rate corrosive liquid environment, using a single corrosion inhibitor product in a range of different flow rates (a wide flow rate range).
Disclosure of Invention
According to the actual needs and defects of the prior corrosion inhibitor applied to the oil field, the corrosion inhibitor composition and the manufacturing method thereof are provided, and the composition has good corrosion prevention effect in the environment of high-speed flowing corrosive liquid or low-speed slow-flow corrosive liquid.
According to one aspect of the invention, there is provided a corrosion inhibitor composition suitable for use in oilfield produced water, the corrosion inhibitor composition comprising the following components: from about 100 parts by weight to 200 parts by weight of an imidazoline component characterized or defined by the following formula:
Figure BDA0002510050090000021
wherein R is1Selected from straight or branched chain hydrocarbon radicals of 3 to 15 carbon atoms; and
from about 30 to 100 parts by weight of an amidothiourea component characterized or defined by the formula:
Figure BDA0002510050090000022
wherein R is2Selected from alkyl groups having 10 to 16 carbon atoms; n is1Is 2, 3 or 4; and
optionally, the corrosion inhibitor composition may further comprise 1 to 20 parts by weight of an auxiliary component.
In an optional aspect, in the corrosion inhibitor composition according to the invention, R1Preferably 3, 4 or 5, said R2Preferably 11, 12 or 13; and said n1Preferably 2.
According to an alternative, in the corrosion inhibitor composition suitable for oilfield produced water of the present invention,
the mass ratio of the components of the formulas 1 and 2 in the corrosion inhibitor composition is 1: (0.3-1), wherein the auxiliary component accounts for no more than 10 wt% of the total corrosion inhibitor composition.
The corrosion inhibitor composition suitable for the oilfield produced water according to any one of the preceding claims, wherein the auxiliary component is one or more selected from organic solvents, water, surfactants and pH regulators; wherein the organic solvent is preferably methanol, ethanol or isopropanol; the surfactant is preferably octyl phenol polyoxyethylene ether; the pH regulator is preferably hydrochloric acid or sodium hydroxide.
In a second aspect of the invention, there is provided a method of making a corrosion inhibitor composition as described above suitable for use in oilfield produced water, the method comprising the steps of:
step 1: adopting trimesic acid to react with methanol, and using concentrated sulfuric acid as a reaction medium to carry out reflux reaction for about 2-5 hours to obtain trimesic acid trimethyl ester;
step 2: dissolving the trimesic acid trimethyl ester in an organic solvent, adding excessive strong base (sodium hydroxide or potassium hydroxide), keeping stirring at the temperature of about 0-5 ℃ under the stirring condition, reacting for about 2-5 hours, washing, and extracting by using hydrochloric acid and chloroform to obtain 3, 5-dicarboxylic acid-1-benzoate;
and step 3: adding alkane amine into the obtained 3, 5-dicarboxylic acid-1-benzoate intermediate product, and carrying out reflux reaction in an organic solvent at the temperature of about 90-140 ℃ for about 3-6 hours to obtain 5- (alkylamine formyl) -1, 3-phthalic acid;
and 4, step 4: adding N-ethyl ethylenediamine into the reaction product of the step 4, and reacting at a temperature of 120 to 150 ℃ for 2 to 4 hours to obtain the component of the formula 1
Figure BDA0002510050090000041
And 5: using alkyl acid with 10 to 16 carbon atoms, diethylenetriamine and thiourea as reactants, adding the raw materials according to the molar ratio of 1:1:1, and carrying out reflux reaction for 4 to 6 hours at the reaction temperature of 90 to 120 ℃ to obtain the component of the formula 2
Figure BDA0002510050090000042
The preparation method comprises the following steps of (1) obtaining an intermediate product by mixing the following components in parts by mass (100-): (30-100): (1-20) mixing to prepare the corrosion inhibitor composition.
In an alternative method, the reaction temperature in step 1 is 40-60 ℃; the reaction temperature in the step 2 is 2-4 ℃; the reaction temperature in the steps 3 and 4 was 120-140 ℃.
In a further alternative method, the mass ratio of the formula 1, the formula 2 and the auxiliary component is 1: (0.3-0.5): (0.1-0.15).
Optionally, the alkane amine is propylamine, butylamine, or pentylamine.
Preferably, the auxiliary component comprises 0.5 wt% to 1 wt% of surfactant, preferably polyoxyethylene octylphenol ether, based on the mass percentage of the whole corrosion inhibitor composition.
The technical solutions and advantages of the present invention will be explained and explained in more detail below with reference to specific embodiments. It should be understood that the contents presented in the description and the detailed description are only for more clearly illustrating the technical solutions and the advantages of the present invention, and do not limit the protection scope of the present invention. On the basis of the disclosure of the specification, a person skilled in the art can modify the technical solution according to various reasonable changes, and the modified technical solution should be understood as being included in the protection scope of the invention as long as the person does not depart from the spirit of the invention.
Detailed Description
The present invention is described in more detail below to facilitate an understanding of the invention.
Before the description of the specific embodiments, the essential fact that part of the main raw materials used have been sourced is described in the present specification. It should be noted that the sources of the raw materials described in the embodiments herein are not limiting, and those skilled in the art can select appropriate raw materials and testing equipment to perform the relevant tests and obtain the corresponding results according to the teaching and teaching of the present invention, and for raw materials which do not describe a specific manufacturer or route, those skilled in the art can select raw materials as the reaction starting materials to meet the corresponding requirements according to the disclosure and requirements of the present specification. It will also be understood from the disclosure of the present specification that the reaction starting materials for the synthesis of a portion of the compounds are derived from the initial product synthesized in the preceding step of the present invention.
Example 1: the invention relates to a synthesis process of a composite corrosion inhibitor composition
Step 1: adopting trimesic acid
Figure BDA0002510050090000051
As one of the raw materials, the method reacts with methanol to prepare methyl trimesate: in the specific manufacturing process, trimesic acid is weighed: the mass ratio of methanol is 1: (3-5) using concentrated sulfuric acid as a reaction medium, wherein the mass ratio of the trimesic acid to the 70 wt% concentrated sulfuric acid is controlled to be 1: (0.05-0.1), controlling the temperature to be 40-60 ℃ to carry out reflux reaction, and controlling the reaction time to be 3 hours; then adjusting the pH value to be neutral, removing impurities and purifying to obtain the methyl trimesate, wherein the methyl trimesate can be represented by the following chemical formula:
Figure BDA0002510050090000052
step 2: dissolving the product of the step 1, namely the methyl ester of trimesic acid in a solvent (excessive methanol), adding an excessive strong base solvent NaOH (or KOH) under the condition of refrigeration (2 ℃), reacting for 2.5 hours under the condition of mechanical stirring, removing the solvent, washing with ethyl acetate, and extracting with hydrochloric acid and chloroform to obtain the methyl ester of trimesic acid, wherein the main component is 3, 5-dicarboxylic acid-1-benzoate:
Figure BDA0002510050090000061
and step 3: using the product (3, 5-dicarboxylic acid-1-benzoate) obtained in step 2, an alkaneamine (propylamine) was added and refluxed at 100 ℃ for 5 hours in a benzene solvent to produce 5- (propylaminoyl) -1, 3-phthalic acid, and the resulting chemical composition was represented by the following formula:
Figure BDA0002510050090000062
in the technical scheme of the inventionParticular classes of alkane amines are optional, optionally amine groups (group-NH-R)1In) R1May be selected from straight chain hydrocarbon groups having 3 to 15 carbon atoms, and propylamine, butylamine or pentylamine is preferably used in the present invention as the alkylamine.
And 4, step 4: on the basis of the product obtained in step 3, the reaction product is reacted with an organic amine (N-ethyl ethylene diamine,
Figure BDA0002510050090000063
) The imidazoline component described in the example is obtained by reacting for 3 hours at 150 ℃ and then dehydrating and cyclizing:
Figure BDA0002510050090000071
and 5: preparing an amidothiourea component:
the preparation of the amidothiourea component requires the use of dodecanoic acid, diethylenetriamine
Figure BDA0002510050090000072
And thiourea. Placing the raw materials into a reflux bottle according to the molar ratio of 1:1:1, setting the reaction temperature at 100 ℃, and carrying out reflux reaction for 5 hours to obtain the amidothiourea component, which can be expressed by the following chemical formula:
Figure BDA0002510050090000073
among the components constituting the composition of this example, 100 parts by weight of the imidazoline component (formula 4) obtained in step 4, 100 parts by weight of the amidothiourea obtained in step 5 (formula 5), and 2 parts by weight of the surfactant octylphenol polyoxyethylene ether were included.
Example 2: corrosion inhibition effect test of corrosion inhibitor components at different fluid speeds
In order to simulate different flow rates in different pipeline environments, different stirrer rotational speeds were used to simulate different fluid velocities in a test experiment for evaluating corrosion inhibitors by a weight loss method. Among them, a corrosion prevention test piece (made of 20# steel) was placed in an autoclave (the inner volume of which was 2500 ml). The test piece was washed with an organic solvent and wiped on the surface for use. The experimental temperature is controlled between 60 ℃ and 90 ℃ and the experimental time is 12 hours. The corrosive medium is circulating water produced by water injection of the petroleum well, and after the acidity of the circulating water is tested, the acidity of the circulating water is adjusted to 12mg/KOH by using naphthenic acid as an auxiliary medium for simulation test. The amount of corrosion inhibitor added is 0.1g/100 g.
The stirrer speed in the autoclave varied from 50 rpm to 1500 rpm.
The corrosion inhibition ratio was calculated according to the following data:
D%=(W0-W1)/W0(ii) a Wherein W0The weight loss value of the steel sheet without any corrosion inhibitor component is expressed in grams (the same unit is below); w1The weight loss value is the weight loss value under the same experimental conditions after the corresponding corrosion inhibitor is added; the D% can be regarded as the proportion of corrosion inhibition after the corrosion effect is improved in comparison with the blank test.
The experimental results of the respective examples and comparative examples are shown in the following table. Wherein example 1 uses the composite corrosion inhibitor composition prepared in the above example. In the blank test, the steel sheet weight loss was measured to be 0.026 g after the test was completed, whereas the steel sheet weight loss was measured to be 0.0031 g under the fluid flow condition of 50 rpm of example 1, as can be obtained from the above formula, and D% was about 88.07%. The calculation of the results of the remaining experiments was similar to the test method described above.
Table 1: corrosion inhibition rate test result obtained by different corrosion inhibitor components
Figure BDA0002510050090000081
In the above table, comparative example 1 used only the imidazoline component used in step 4; comparative example 2 only the amidothiourea component obtained in step 5 referred to in example 1 of the present invention was used. The experimental conditions used for examples 3-5 are described below.
From the experimental comparison, the composite corrosion inhibitor composition provided by the invention achieves more excellent corrosion inhibition effect in the environment with low fluid flow speed and ultrahigh fluid flow speed. Although both comparative examples 1 and 2 achieved corrosion inhibition greater than 70% as specified in the industry specifications (Q/SHCG40-2012), each component alone did not achieve excellent corrosion inhibition over the full fluid velocity.
The inventors do not wish to be bound by any theory or explanation. However, the inventor believes through research and experiments that one possible explanation is that the imidazoline component synthesized by the invention has more active centers to facilitate film formation, thus has better film forming property under high fluidity, but can be deposited to form a film slowly under low flow rate because of the structure of the imidazoline component tending to be cyclic; after the corrosion inhibitor is combined with the amido thiourea basically in a linear structure state, the linear structure drives or is combined or connected with the imidazoline component with a cyclic structure, so that the corrosion inhibitor component is actively deposited to form a film at a low flow rate, and the film forming property and the corrosion inhibition effect are improved.
Example 3: the corrosion inhibitor composition of the invention with different component ratios
The different example schemes resulting from the adjustment of the different imidazoline, amidothiourea, and auxiliary components according to the inventive concept are as follows, as shown in table 1, which achieve the improved corrosion inhibition over a wide range of fluid velocities as in example 1.
Table 2: corrosion inhibition rate test result obtained by different corrosion inhibitor components
Figure BDA0002510050090000091
From the above comparison, it can be seen that the surfactant content in example 2 is increased relative to that in example 1, but slightly worse corrosion inhibition is achieved at lower fluid flow rates than in example 1. The inventors believe that the surfactant content in the preferred embodiment of the present invention should be less than 2 wt% of the main component (the sum of the imidazoline component and the amidothiourea), which may help to achieve a balance of the activity of the high molecular component and the film forming deposition characteristics, and when the surfactant content is too high, the film forming and corrosion preventing characteristics may be degraded. In contrast, in example 4, which does not contain a surfactant, it seems that the corrosion inhibition effect at high fluid fluidity is slightly reduced, and therefore, it is preferable to contain a smaller amount of the surfactant. From experimental observation, the organic solvent is helpful for the intermixing storage performance of the corrosion inhibitor composition, but the effect in practical use has little influence.
According to the embodiments and technical contents described in the present specification, the present invention can provide at least the following technical means: while the present disclosure includes specific embodiments, it will be apparent to those skilled in the art that various substitutions or alterations in form and detail may be made to these embodiments without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents. The embodiments described herein are to be considered in all respects only as illustrative and not restrictive. The description of features and aspects in each embodiment is believed to be applicable to similar features and aspects in other embodiments. Therefore, the scope of the present disclosure should be defined not by the detailed description but by the claims, and all changes within the scope of the claims and equivalents thereof should be construed as being included in the technical solution of the present disclosure.
The invention at least provides the following technical scheme:
scheme 1: a corrosion inhibitor composition suitable for use in oilfield produced water, the corrosion inhibitor composition comprising:
from about 100 parts by weight to 200 parts by weight of an imidazoline component characterized or defined by the following formula:
Figure BDA0002510050090000101
wherein R is1Selected from straight or branched chain hydrocarbon radicals of 3 to 15 carbon atoms; and
from about 30 to 100 parts by weight of an amidothiourea component characterized or defined by the formula:
Figure BDA0002510050090000111
wherein R is2Selected from alkyl groups having 10 to 16 carbon atoms; n is1Is 2, 3 or 4; and
optionally, the corrosion inhibitor composition may further comprise 1 to 20 parts by weight of an auxiliary component.
Scheme 2: the corrosion inhibitor composition suitable for oilfield produced water according to the scheme is characterized in that R is1Preferably 3, 4 or 5, said R2Preferably 11, 12 or 13; and said n1Preferably 2.
Scheme 3: the corrosion inhibitor composition suitable for the oilfield produced water according to the scheme is characterized in that,
the mass ratio of the components of the formulas 1 and 2 in the corrosion inhibitor composition is 1: (0.3-1), wherein the auxiliary component accounts for no more than 10 wt% of the total corrosion inhibitor composition.
Scheme 4: the corrosion inhibitor composition suitable for the oilfield produced water according to the scheme is characterized in that,
the auxiliary component is selected from one or more of organic solvent, water, surfactant and pH value regulator; wherein the organic solvent is preferably methanol, ethanol or isopropanol; the surfactant is preferably octyl phenol polyoxyethylene ether; the pH regulator is preferably hydrochloric acid or sodium hydroxide.
Scheme 5: a method for preparing a corrosion inhibitor composition suitable for oilfield produced water according to any one of the preceding claims, the method comprising the steps of:
step 1: adopting trimesic acid to react with methanol, and using concentrated sulfuric acid as a reaction medium to carry out reflux reaction for about 2-5 hours to obtain trimesic acid trimethyl ester;
step 2: dissolving the methyl ester of trimesic acid in an organic solvent, adding excessive strong base, keeping stirring and reacting for about 2-5 hours at the temperature of about 0-5 ℃ under the stirring condition, washing, and extracting by using hydrochloric acid and chloroform to obtain 3, 5-dicarboxylic acid-1-benzoate;
and step 3: adding alkane amine into the obtained 3, 5-dicarboxylic acid-1-benzoate intermediate product, and carrying out reflux reaction in an organic solvent at the temperature of about 90-140 ℃ for about 3-6 hours to obtain 5- (alkylamine formyl) -1, 3-phthalic acid;
and 4, step 4: adding N-ethyl ethylenediamine into the reaction product of the step 4, and reacting at a temperature of 120 to 150 ℃ for 2 to 4 hours to obtain the component of the formula 1
Figure BDA0002510050090000121
And 5: using alkyl acid with 10 to 16 carbon atoms, diethylenetriamine and thiourea as reactants, adding the raw materials according to the molar ratio of 1:1:1, and carrying out reflux reaction for 4 to 6 hours at the reaction temperature of 90 to 120 ℃ to obtain the component of the formula 2
Figure BDA0002510050090000122
The preparation method comprises the following steps of (1) obtaining an intermediate product by mixing the following components in parts by mass (100-): (30-100): (1-20) mixing to prepare the corrosion inhibitor composition.
Scheme 6: the method of claim 5,
the reaction temperature in the step 1 is 40-60 ℃;
the reaction temperature in the step 2 is 2-4 ℃;
the reaction temperature in the steps 3 and 4 was 120-140 ℃.
Scheme 7: the method according to the preceding aspect, characterized in that,
the mass ratio of the formula 1 to the formula 2 to the auxiliary group is 1: (0.3-0.5): (0.1-0.15).
Scheme 8: the method according to the preceding aspect, wherein the alkane amine is propylamine, butylamine or pentylamine.
Scheme 9: the method according to the previous scheme, characterized in that the auxiliary component comprises 0.5-1 wt% of surfactant, preferably octylphenol polyoxyethylene ether, based on the mass percentage of the whole corrosion inhibitor composition.

Claims (9)

1. A corrosion inhibitor composition suitable for use in oilfield produced water, the corrosion inhibitor composition comprising:
from about 100 parts by weight to 200 parts by weight of an imidazoline component characterized or defined by the following formula:
Figure FDA0002510050080000011
wherein R is1Selected from straight or branched chain hydrocarbon radicals of 3 to 15 carbon atoms; and
from about 30 to 100 parts by weight of an amidothiourea component characterized or defined by the formula:
Figure FDA0002510050080000012
wherein R is2Selected from alkyl groups having 10 to 16 carbon atoms; n is1Is 2, 3 or 4; and
optionally, the corrosion inhibitor composition may further comprise 1 to 20 parts by weight of an auxiliary component.
2. The corrosion inhibitor composition suitable for oilfield produced water of claim 1, wherein R is R1Preferably 3, 4 or 5, said R2Preferably 11, 12 or 13; and said n1Preferably 2.
3. The corrosion inhibitor composition suitable for oilfield produced water according to any of the preceding claims, wherein the corrosion inhibitor composition comprises a metal selected from the group consisting of aluminum, nickel, copper, nickel,
the mass ratio of the components represented by the formulas 1 and 2 in the corrosion inhibitor composition is 1: (0.3-1), wherein the auxiliary component accounts for no more than 10 wt% of the total corrosion inhibitor composition.
4. The corrosion inhibitor composition suitable for oilfield produced water according to any of the preceding claims, wherein the corrosion inhibitor composition comprises a metal selected from the group consisting of aluminum, nickel, copper, nickel,
the auxiliary component is selected from one or more of organic solvent, water, surfactant and pH value regulator; wherein the organic solvent is preferably methanol, ethanol or isopropanol; the surfactant is preferably octyl phenol polyoxyethylene ether; the pH regulator is preferably hydrochloric acid or sodium hydroxide.
5. A method of preparing a corrosion inhibitor composition suitable for use in oilfield produced water according to any one of claims 1 to 4, the method comprising the steps of:
step 1: adopting trimesic acid to react with methanol, and using concentrated sulfuric acid as a reaction medium to carry out reflux reaction for about 2-5 hours to obtain trimesic acid trimethyl ester;
step 2: dissolving the trimesic acid trimethyl ester in an organic solvent, adding excessive strong base, keeping stirring and reacting for about 2-5 hours at the temperature of about 0-5 ℃ under the stirring condition, washing, and extracting by adopting hydrochloric acid and chloroform to obtain 3, 5-dicarboxylic acid-1-benzoate;
and step 3: adding alkane amine into the obtained 3, 5-dicarboxylic acid-1-benzoate intermediate product, and carrying out reflux reaction in an organic solvent at the temperature of about 90-140 ℃ for about 3-6 hours to obtain 5- (alkylamine formyl) -1, 3-phthalic acid;
and 4, step 4: adding N-ethyl ethylenediamine into the reaction product of the step 4, and reacting at a temperature of 120 to 150 ℃ for 2 to 4 hours to obtain the component of the formula 1
Figure FDA0002510050080000021
And 5: using alkyl acid with 10 to 16 carbon atoms, diethylenetriamine and thiourea as reactants, adding the raw materials according to the molar ratio of 1:1:1, and carrying out reflux reaction for 4 to 6 hours at the reaction temperature of 90 to 120 ℃ to obtain the productTo the component of said formula 2
Figure FDA0002510050080000031
The preparation method comprises the following steps of (1) obtaining an intermediate product by mixing the following components in parts by mass (100-): (30-100): (1-20) mixing to prepare the corrosion inhibitor composition.
6. The method of claim 5,
the reaction temperature in the step 1 is 40-60 ℃;
the reaction temperature in the step 2 is 2-4 ℃;
the reaction temperature in the steps 3 and 4 was 120-140 ℃.
7. The method according to claim 5 or 6,
the mass ratio of the formula 1 to the formula 2 to the auxiliary components is 1: (0.3-0.5): (0.1-0.15).
8. The process according to any one of claims 5 to 7, characterized in that the alkane amine is propylamine, butylamine or pentylamine.
9. The method according to any one of claims 5 to 8, wherein the auxiliary component comprises 0.5 to 1 wt% of a surfactant, preferably octylphenol polyoxyethylene ether, based on the mass percentage of the total corrosion inhibitor composition.
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Publication number Priority date Publication date Assignee Title
CN116535635A (en) * 2023-07-05 2023-08-04 四川省工业环境监测研究院 Schiff base, preparation method thereof and corrosion inhibitor for oil and gas well
CN116535635B (en) * 2023-07-05 2023-09-01 四川省工业环境监测研究院 Schiff base, preparation method thereof and corrosion inhibitor for oil and gas well

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