CN110952100A - Oil-soluble corrosion inhibitor for gathering pipeline pre-film and preparation method thereof - Google Patents
Oil-soluble corrosion inhibitor for gathering pipeline pre-film and preparation method thereof Download PDFInfo
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- CN110952100A CN110952100A CN201811126811.0A CN201811126811A CN110952100A CN 110952100 A CN110952100 A CN 110952100A CN 201811126811 A CN201811126811 A CN 201811126811A CN 110952100 A CN110952100 A CN 110952100A
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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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/04—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D233/06—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/04—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D233/06—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
- C07D233/08—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms with alkyl radicals, containing more than four carbon atoms, directly attached to ring carbon atoms
- C07D233/12—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms with alkyl radicals, containing more than four carbon atoms, directly attached to ring carbon atoms with substituted hydrocarbon radicals attached to ring nitrogen atoms
- C07D233/16—Radicals substituted by nitrogen atoms
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Abstract
The invention relates to an oil-soluble corrosion inhibitor for gathering pipeline pre-film and a preparation method thereof, wherein the corrosion inhibitor comprises the following components in percentage by mass: 20-30% of main agent and 70-80% of compound; the primary agent is composed of a first imidazoline and a second imidazoline, the first imidazoline has a formula [1]The second imidazoline has the formula [2]]The structure of (1). The corrosion inhibitor has strong oil solubility, can improve the plane spreadability of corrosion inhibitor molecules on the metal surface, forms a multi-layer net-shaped compact protective film, prevents corrosive liquid from contacting with a metal matrix, achieves the aim of efficient corrosion prevention, and can be used for H-containing2S/CO2The carbon steel pipeline and equipment in the environment of the gas gathering and transportation pipeline have good protection effect.
Description
Technical Field
The invention relates to a corrosion inhibitor preparation technology, in particular to an oil-soluble corrosion inhibitor for a gathering pipeline pre-film and a preparation method thereof, belonging to the technical field of petroleum and petrochemical gathering pipelines and equipment protection.
Background
Corrosion inhibitor corrosion prevention is one of corrosion prevention measures which are generally adopted in the petroleum and petrochemical fields at home and abroad and have good effect, and corrosion inhibitor pipe cleaning pre-film is a mode which is widely applied in corrosion inhibitor corrosion prevention measures. The mode can not only carry out all-around coating of the corrosion inhibitor on the inner surface of the pipeline in time after cleaning the pipeline, but also avoid the practical problem that the carrying distance of the corrosion inhibitor can not meet the requirement under the condition that the liquid amount in the medium in the pipeline is less.
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 is mainly imidazoline and derivatives thereof, polyol phosphate and the like, and the dosage of the imidazoline and the derivatives thereof is the largest due to the advantages of small dosage, excellent corrosion inhibition performance and the like.
For example, CN102234502B discloses a corrosion inhibitor and a preparation method thereof, and CN100591803C discloses an anti-H2S/CO2The corrosion inhibitor under the combined action and CN101705112A disclose a water-soluble imidazoline amide corrosion inhibitor and a preparation method thereofIn the application method, the corrosion inhibitor in the application documents is a water-soluble corrosion inhibitor, and does not have the oil-soluble corrosion inhibitor similar to the related oil-soluble corrosion inhibitor for pigging and pre-filming.
Compared with the water-soluble corrosion inhibitor, the oil-soluble corrosion inhibitor has better adsorbability on the metal surface, and is mainly characterized in that:
the nitrogen atom in the imidazoline molecule has a lone pair electron, and the lone pair electron can enter a dsp hollow track hybridized by an iron atom (ion) to form a coordination bond, and a complexing action is carried out to generate a stable chelate with a six-membered ring structure to be adsorbed on the iron surface to form a complete plane hydrophobic protective film, so that the anode process of corrosion reaction of the iron ion of a corrosion product diffusing into the solution is prevented, and the corrosion reaction speed is slowed down; double bonds in the alkyl chain and surrounding atoms generate a conjugation effect to form delocalized big pi bonds, and the big pi bonds are easy to interact with d empty orbitals of iron atoms on the surface of the metal to form coordination bonds, so that the further adsorption of imidazoline molecules on the surface of the metal is enhanced; and secondly, alkyl chain molecules and oil-soluble solvents such as diesel oil have the effect of 'similar compatibility', and the better solubility and dispersibility further improve the planar spreadability of the corrosion inhibitor molecules on the metal surface. Meanwhile, the corrosion inhibitor is further mutually promoted and supplemented with other auxiliary agents to be adsorbed on the metal surface together to form a multi-layer net-shaped compact protective film to prevent the corrosion liquid from contacting with the metal matrix, so that the aim of high-efficiency corrosion prevention is fulfilled.
Therefore, how to prepare the oil-soluble corrosion inhibitor for pigging and pre-filming of gathering pipelines is a technical problem to be solved urgently in the field.
Disclosure of Invention
The invention provides an oil-soluble corrosion inhibitor for gathering pipeline pre-film and a preparation method thereof, the corrosion inhibitor has stronger oil solubility, can improve the planar spreading property of corrosion inhibitor molecules on the metal surface, forms a multi-layer net-shaped compact protective film, prevents corrosive liquid from contacting with a metal matrix, achieves the aim of high-efficiency corrosion prevention, and can be used for H-containing corrosion prevention2S/CO2The carbon steel pipeline and equipment in the environment of the gas gathering and transportation pipeline have good protection effect.
The invention provides an oil-soluble corrosion inhibitor for gathering pipeline pre-film, which comprises the following components in percentage by mass: 20-30% of main agent and 70-80% of compound;
the main agent is composed of a first imidazoline and a second imidazoline, the first imidazoline has a structure of a formula [1], the second imidazoline has a structure of a formula [2],
wherein n is not less than 1 and is a natural number, R1And R2Independently selected from the formula [3]-formula [8]A group represented by, and R1And R2Are different from each other;
"" indicates a bond.
The invention also provides an oil-soluble corrosion inhibitor for the gathering pipeline pre-film, which comprises the following components in percentage by mass: 20-30% of main agent and 70-80% of compound; wherein the content of the first and second substances,
the main agent is a product collected when the acid value of a reaction system is less than 5mg/kg after the amidation reaction of organic acid and polyamine substances and the heat preservation at 220 ℃ of 170-; the organic acid comprises two of capric acid, myristic acid, behenic acid, erucic acid, eleostearic acid and abietic acid, the polyamine substance is selected from diethylenetriamine, tetraethylenepentamine or polyethylene polyamine, and the ratio of the sum of the moles of the two organic acids to the moles of the amine substance is 1: (1.2-1.5).
The corrosion inhibitor is characterized in that in the process of preparing the main agent, one of the organic acids is eleostearic acid, and the molar ratio of the eleostearic acid to the other organic acid is 1 (2-5); or the organic acid comprises two of capric acid, myristic acid, behenic acid, erucic acid and abietic acid, and the molar ratio of the two acids is 1: 1.
The corrosion inhibitor as described above, wherein the compound comprises the following components by weight: 10-15% of alkylamine, 5-19% of phosphate and 45% -65% of solvent.
The corrosion inhibitor as described above, wherein the alkylamine is selected from one of dodecylamine, hexadecylamine and octadecylamine.
The corrosion inhibitor as described above, wherein the phosphate ester is selected from one of polyoxyethylene alkylphenol ether phosphate ester, isotridecanol phosphate ester and isotridecanol ether phosphate ester.
The invention also provides a preparation method of any one of the corrosion inhibitors, which comprises the following steps:
mixing two organic acids and polyamine substances to carry out amidation reaction, and keeping the temperature of the amidation product system at 170-220 ℃ for more than 1 hour to ensure that the acid value of the reaction system is less than 5mg/kg to obtain the main agent;
at room temperature, mixing the main agent and the compound and uniformly stirring to obtain the corrosion inhibitor;
alternatively, the first and second electrodes may be,
mixing two organic acids with polyamine substances respectively to perform amidation reaction, keeping the temperature of an amidation product system at 170-220 ℃ for more than 1 hour to ensure that the acid value of the reaction system is less than 5mg/kg, and mixing the two reaction products to obtain the main agent;
and (3) mixing the main agent and the compound at room temperature, and uniformly stirring to obtain the corrosion inhibitor.
The preparation method comprises the steps of using xylene as a solvent for amidation reaction, raising the temperature to 150-160 ℃, and maintaining the reaction time for 1-5 hours;
and heating the amidation product system to 170-180 ℃ for continuous reaction for 1-2h, then heating to 210-220 ℃ for heat preservation for 2-5h, and obtaining the main agent when the acid value of the reaction system is less than 5 mg/kg.
The production process as described above, wherein the rate of temperature rise is controlled to be not higher than 20 ℃/10m2 n.
The implementation of the invention has at least the following advantages:
1. the corrosion inhibitor has simple components, stable system and convenient use, and can effectively prevent the gathering and transportation pipeline from being corroded;
2. the corrosion inhibitor has good oil solubility, can generate stable chelate with a six-membered ring structure to be adsorbed on the surface of iron to form a complete plane hydrophobic protective film, thereby preventing the anode process of corrosion reaction of iron ions of a corrosion product diffusing into a solution, slowing down the corrosion reaction speed, further enhancing the corrosion inhibition effect and having strong practicability;
3. the oil solubility of the corrosion inhibitor is also beneficial to improving the planar spreadability of corrosion inhibitor molecules on the metal surface, forming a multi-layer net-shaped compact protective film, and preventing the corrosion liquid from contacting with a metal matrix, thereby achieving the purpose of high-efficiency corrosion prevention;
4. the preparation method of the corrosion inhibitor is simple to operate and easy to control, and is not only favorable for forming a stable corrosion inhibitor system, but also favorable for using the corrosion inhibitor.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides an oil-soluble corrosion inhibitor for gathering pipeline pre-film, which comprises the following components in percentage by mass: 20-30% of main agent and 70-80% of compound;
the main agent is composed of a first imidazoline and a second imidazoline, the first imidazoline has a structure of a formula [1], the second imidazoline has a structure of a formula [2],
wherein n is not less than 1 and is a natural number, R1And R2Independently selected from the formula [3]-formula [8]A group represented by, and R1And R2Are different from each other;
"" indicates a bond.
The corrosion inhibitor provided by the invention has simple composition, does not generate layering and precipitation and has stable state. The main agent is a mixture of the first imidazoline and the second imidazoline. Compared with imidazoline which is used as the main functional component of the corrosion inhibitor, the corrosion inhibitor adopts the first imidazoline and the second imidazoline which are mixed as the main functional component of the corrosion inhibitor, so that the film forming firmness of the corrosion inhibitor on the inner wall of the gathering pipeline can be enhanced, and the corrosion inhibiting effect of the corrosion inhibitor on the gathering pipeline is obviously improved.
Wherein, if R1Or R2Is of the formula [4]In the structure shown, for example, R1Is of the formula [4]The structure is shown, the molar ratio of the first imidazoline to the second imidazoline is 1: (2-5); on the contrary, if R2Is of the formula [4]The structure shown, the molar ratio of the first imidazoline to the second imidazoline is (2-5): 1;
if R is1And R2Is not of the formula [4]In the structure shown, the molar ratio of the first imidazoline to the second imidazoline is 1: 1.
meanwhile, based on the total weight of the corrosion inhibitor, the compound comprises the following components in percentage by mass:
10-15% of alkylamine, 5-19% of phosphate and 45% -65% of solvent.
Namely, the corrosion inhibitor comprises the following components in percentage by mass: 20-30% of main agent, 10-15% of alkylamine, 5-19% of phosphate and 45-65% of solvent.
In addition, the invention also provides an oil-soluble corrosion inhibitor for gathering pipeline pre-film, which comprises the following components in percentage by mass: 20-30% of main agent and 70-80% of compound; wherein the main agent is a product collected when the acid value of a reaction system is less than 5mg/kg after the amidation reaction of organic acid and polyamine substances and the heat preservation at 220 ℃ of 170-; the organic acid comprises two of capric acid, myristic acid, behenic acid, erucic acid, eleostearic acid and abietic acid, the polyamine is selected from diethylenetriamine, tetraethylenepentamine or polyethylene polyamine, and the ratio of the sum of the mole numbers of the two organic acids to the mole number of the polyamine is 1: (1.2-1.5).
The corrosion inhibitor comprises a main agent and a compound in the proportion, wherein the main agent is obtained by carrying out amidation reaction on organic acid and polyamine substances and then dehydrating at a certain temperature to form a ring.
In the corrosion inhibitor of the present invention, the preparation method of the main agent constituting the corrosion inhibitor is not particularly limited, and for example, the corrosion inhibitor may be obtained by mixing two organic acids and then reacting with polyamine substances and then performing a correlation reaction, or may be obtained by separately reacting two organic acids with polyamine substances and then performing a correlation reaction, and finally mixing the two products.
Further, the ratio between the two organic acids during the preparation of the main agent varies depending on the specific selection of the two organic acids.
Specifically, if one of the organic acids is eleostearic acid, the molar ratio of eleostearic acid to the other organic acid is 1 (2-5); if one of the two organic acids is not eleostearic acid, that is, the organic acid is selected from two of capric acid, myristic acid, behenic acid, erucic acid and abietic acid, the molar ratio of the two organic acids is 1: 1.
Further, based on the total weight of the corrosion inhibitor, the compound comprises the following components in percentage by mass:
10-15% of alkylamine, 5-19% of phosphate and 45% -65% of solvent.
Namely, the corrosion inhibitor comprises the following components in percentage by mass: 20-30% of main agent, 10-15% of alkylamine, 5-19% of phosphate and 45-65% of solvent.
In the compound, the alkylamine is selected from one of dodecylamine, hexadecylamine and octadecylamine; the phosphate is selected from one of polyoxyethylene alkyl phenol ether phosphate, isotridecanol phosphate and isotridecanol ether phosphate; the solvent is selected from one or two of diesel oil and solvent oil, and the invention does not limit the mixing ratio of each component of the solvent.
Wherein, the solvent oil can be further selected from one of solvent oil 100#, solvent oil 150#, and solvent oil 200 #.
The invention also provides a preparation method of any one of the corrosion inhibitors, which comprises the following steps:
mixing two organic acids and polyamine substances to carry out amidation reaction, and keeping the temperature of the amidation product system at 170-220 ℃ for more than 1 hour to ensure that the acid value of the reaction system is less than 5mg/kg to obtain a main agent;
mixing the main agent and the compound at room temperature, and uniformly stirring to obtain the corrosion inhibitor;
alternatively, the first and second electrodes may be,
mixing two organic acids with polyamine substances respectively to perform amidation reaction, continuously preserving the temperature of an amidation product system at 170-220 ℃ for more than 1 hour to ensure that the acid value of the reaction system is less than 5mg/kg, and mixing the two reaction products to obtain a main agent;
and (3) mixing the main agent and the compound at room temperature, and uniformly stirring to obtain the corrosion inhibitor.
The corrosion inhibitor is prepared by two preparation methods, wherein the two preparation methods are substantially the same, and two amide products are obtained by firstly carrying out amidation reaction on two organic acids and polyamine substances; then dehydrating the two amide products into rings, wherein the mixture of the products after dehydration and cyclization of the two amide products is the main agent; finally, the main agent and the compound are mixed according to a limited proportion to obtain the corrosion inhibitor. The difference is that the first is that two acids are mixed and then reacted, and the second is that the two acids are respectively reacted, and finally the products are mixed. In addition, the main agent, alkylamine, phosphate and solvent can be mixed and stirred uniformly according to the proportion to obtain the corrosion inhibitor without preparing a compound in advance.
In the two preparation methods, the two organic acids are respectively selected from capric acid, myristic acid, behenic acid, erucic acid, eleostearic acid and abietic acid, and the two organic acids are different; the polyamine substance is selected from diethylenetriamine, tetraethylenepentamine or polyethylene polyamine, and the ratio of the sum of the moles of the two organic acids to the moles of the polyamine substance is 1: (1.2-1.5).
It is to be noted that the ratio between the two organic acids during the preparation of the main agent varies according to the specific choice of the two organic acids.
Specifically, if one of the organic acids is eleostearic acid, the molar ratio of eleostearic acid to the other organic acid is 1: (2-5); if one of the two organic acids is not eleostearic acid, that is, the organic acid is selected from two of capric acid, myristic acid, behenic acid, erucic acid and abietic acid, the molar ratio of the two organic acids is 1: 1.
Further, the amidation reaction uses xylene as solvent, the temperature is raised to 150-; the amidation product system needs no post treatment, and is directly heated to 170-180 ℃ for continuous reaction for 1-2h, then is heated to 210-220 ℃ for heat preservation for 2-5h, and when the acid value of the reaction system is less than 5mg/kg, the main agent is obtained. Wherein, the temperature rising rate is controlled not to be higher than 20 ℃/10m < 2 > 2n, otherwise, side reaction can occur when the temperature rises too fast.
Specifically, amidation of two organic acids with polyamines to form R1And R2Wherein xylene acts as a water-carrying agent and the mass of xylene is 10% of the total mass of the two organic acids and the polyamine species.
Taking polyamine substances such as diethylenetriamine and tetraethylenepentamine as examples, the reaction equation of amidation is as follows (wherein, when the amine substance is diethylenetriamine, n is 1; and when the amine substance is tetraethylenepentamine, n is 3):
wherein the content of the first and second substances,
when one of the two organic acids is abietic acid, then R1Or R2Is of the formula [3]A group shown;
when one of the two organic acids is eleostearic acid, then R is1Or R2Is of the formula [4]A group shown;
when one of the two organic acids isWhen it is erucic acid, then R1Or R2Is of the formula [5]A group shown;
when one of the two organic acids is behenic capric acid, then R1Or R2Is of the formula [6]A group shown;
when one of the two organic acids is capric acid, then R1Or R2Is of the formula [7]A group shown;
when one of the two organic acids is myristic acid, then R1Or R2Is of the formula [8]A group shown;
in practical operation, the organic acid and the polyamine substance can be added into the reaction kettle, then the xylene is added, and along with the increase of the temperature and the continuation of the heat preservation process, water flows out of a condensation pipe of the reaction kettle, namely, the amidation reaction is carried out at the moment.
The amide generated by the reaction is continuously dehydrated and cyclized to generate R along with the continuous increase of the temperature and the heat preservation1And R2Imidazoline of (4).
Specifically, the reaction equation for imidazoline formation is as follows:
it should be noted that, after the incubation for 2-5h, the acid value of the reaction system needs to be checked, and when the acid value is less than 5mg/kg, the reaction is fully performed, so as to obtain the main agent of the present invention. In specific operation, the reaction system may be cooled to 50 ℃ and then sampled to detect the acid value.
The corrosion inhibitor and the preparation method of the present invention are described in detail below by way of several examples.
Example 1
The preparation method of the corrosion inhibitor of the embodiment comprises the following steps: .
1) Mixing a mixture of two organic acids and diethylenetriamine according to a molar ratio of 1: 1.5 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n; wherein, the two organic acids are eleostearic acid and abietic acid, and the molar ratio of eleostearic acid to abietic acid is 1: 4;
in the reaction process, water flows out of a condensation pipe at the top of the reaction kettle, and the generated acid amide of eleostearic acid and the acid amide of abietic acid;
2) continuously heating to 170 ℃ and 180 ℃, reacting for 1.5h, then continuously heating to 210 ℃ and 220 ℃, preserving the heat for 4h at the temperature, and heating at the speed of not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5mg/kg, and the main agent, namely the mixture of eleostearic acid imidazoline and abietic acid imidazoline is obtained;
3) then, the oil-soluble corrosion inhibitor for gathering and transportation pipeline pre-film of the embodiment is obtained by uniformly mixing 25 mass percent of main agent (mixture of eleostearic acid imidazoline and abietic acid imidazoline), 10 mass percent of octadecylamine, 7 mass percent of polyoxyethylene alkylphenol ether phosphate and 200#58 mass percent of solvent oil, and the code TLM-YM-01 is obtained.
Example 2
The preparation method of the corrosion inhibitor of the embodiment comprises the following steps:
1) mixing a mixture of two organic acids and diethylenetriamine according to a molar ratio of 1: 1.3 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n; wherein, the two organic acids are erucic acid and abietic acid, and the molar ratio of the erucic acid to the abietic acid is 1: 1;
in the reaction process, water flows out from a condensation pipe at the top of the reaction kettle, and the generated acid amide of the erucic acid and the acid amide of the abietic acid;
2) continuously heating to 170 ℃ and 180 ℃, reacting for 1.5h, then continuously heating to 210 ℃ and 220 ℃, preserving the heat for 4h at the temperature, and heating at the speed of not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5mg/kg, and the main agent, namely the mixture of erucic acid imidazoline and abietic acid imidazoline is obtained;
3) then, the main agent (mixture of erucic acid imidazoline and abietic acid imidazoline) is 20 percent, the hexadecylamine is 15 percent, the isotridecanol ether phosphate is 10 percent, and the solvent oil is 150#55 percent, so as to obtain the oil-soluble corrosion inhibitor for the gathering pipeline pre-film of the embodiment, the code TLM-YM-02.
Example 3
The preparation method of the corrosion inhibitor of the embodiment comprises the following steps:
1) mixing a mixture of two organic acids and diethylenetriamine according to a molar ratio of 1: 1.2 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n; wherein, the two organic acids comprise myristic acid and behenic acid, and the molar ratio of the myristic acid to the behenic acid is 1: 1;
in the reaction process, water flows out from a condensation pipe at the top of the reaction kettle, and the amide of myristic acid and the amide of behenic acid are generated at the moment;
2) continuously heating to 170 ℃ and 180 ℃, reacting for 1.5h, then continuously heating to 210 ℃ and 220 ℃, preserving the heat for 4h at the temperature, and heating at the speed of not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5mg/kg, and the main agent, namely the mixture of the myristic acid imidazoline and the behenic acid imidazoline is obtained.
3) Then, the main agent (the mixture of myristic acid imidazoline and behenic acid imidazoline) is 20 percent, the dodecylamine is 10 percent, the isotridecanol ether phosphate ester is 5 percent, and the solvent oil is 100#65 percent, and the oil-soluble corrosion inhibitor for the gathering and transportation pipeline pre-film of the embodiment is obtained, and the code is TLM-YM-03.
Example 4
The preparation method of the corrosion inhibitor of the embodiment comprises the following steps:
1) mixing capric acid and diethylenetriamine according to a molar ratio of 0.5: 1.5 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n;
in the reaction process, water flows out from a condensation pipe at the top of the reaction kettle, and the generated amide of the decanoic acid; heating to 170 ℃ and 180 ℃, continuing to heat to 210 ℃ and 220 ℃ after reacting for 1.5h, and keeping the temperature for 4h at the temperature, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5 mg/kg;
2) mixing behenic acid and diethylenetriamine according to a molar ratio of 0.5: 1.5 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n;
in the reaction process, water flows out from a condensation pipe at the top of the reaction kettle, and the generated acid amide of the behenic acid; heating to 170 ℃ and 180 ℃, continuing to heat to 210 ℃ and 220 ℃ after reacting for 1.5h, and keeping the temperature for 4h at the temperature, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5 mg/kg;
3) mixing the reaction systems obtained in the steps 1) and 2) to obtain a main agent (a mixture of decanoic acid imidazoline and behenic acid imidazoline);
then, uniformly mixing 30% of main agent, 10% of octadecylamine, 10% of isotridecanol phosphate and 50% of diesel oil by mass percentage to obtain the oil-soluble corrosion inhibitor for gathering pipeline pre-film of the embodiment with the code TLM-YM-04.
Example 5
The preparation method of the corrosion inhibitor of the embodiment comprises the following steps:
1) mixing a mixture of two organic acids and diethylenetriamine according to a molar ratio of 1: 1.5 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n; wherein, the two organic acids are capric acid and erucic acid, and the molar ratio of the capric acid to the erucic acid is 1: 1;
in the reaction process, water flows out from a condensation pipe at the top of the reaction kettle, and the generated amide of the capric acid and the amide of the erucic acid;
2) continuously heating to 170 ℃ and 180 ℃, reacting for 1.5h, then continuously heating to 210 ℃ and 220 ℃, preserving the heat for 4h at the temperature, and heating at the speed of not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5mg/kg, and the main agent, namely the mixture of the decanoic acid imidazoline and the erucic acid imidazoline is obtained.
3) Then, uniformly mixing 20% of main agent (mixture of decanoic acid imidazoline and erucic acid imidazoline), 15% of octadecylamine, 10% of polyoxyethylene alkylphenol ether phosphate and 55% of diesel oil by mass percentage to obtain the oil-soluble corrosion inhibitor for gathering and transportation pipeline pre-film of the embodiment, the code TLM-YM-05.
Example 6
The preparation method of the corrosion inhibitor of the embodiment comprises the following steps:
1) mixing a mixture of two organic acids and diethylenetriamine according to a molar ratio of 1: 1.5 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n; wherein, the two organic acids are capric acid and eleostearic acid, and the molar ratio of the capric acid to the eleostearic acid is 7: 3;
in the reaction process, water flows out of a condensation pipe at the top of the reaction kettle, and the generated acid amide of the capric acid and the acid amide of the eleostearic acid;
2) continuously heating to 170 ℃ and 180 ℃, reacting for 1.5h, then continuously heating to 210 ℃ and 220 ℃, preserving the heat for 4h at the temperature, and heating at the speed of not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5mg/kg, and the main agent, namely the mixture of the decanoic acid imidazoline and the eleostearic acid imidazoline is obtained.
3) Then, uniformly mixing 25% of a main agent (a mixture of decanoic acid imidazoline and eleostearic acid imidazoline), 15% of dodecylamine, 6% of polyoxyethylene alkylphenol ether phosphate and 54% of diesel oil by mass percentage to obtain the oil-soluble corrosion inhibitor for the gathering and transportation pipeline pre-film of the embodiment with the code TLM-YM-06.
Example 7
The preparation method of the corrosion inhibitor of the embodiment comprises the following steps:
1) mixing a mixture of two organic acids and diethylenetriamine according to a molar ratio of 1: 1.5 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n; wherein, the two organic acids are behenic acid and abietic acid, and the molar ratio of the behenic acid to the abietic acid is 1: 1;
in the reaction process, water flows out from a condensation pipe at the top of the reaction kettle, and the generated acid amide of the behenic acid and the acid amide of the abietic acid;
2) continuously heating to 170 ℃ and 180 ℃, reacting for 1.5h, then continuously heating to 210 ℃ and 220 ℃, preserving the heat for 4h at the temperature, and heating at the speed of not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5mg/kg, and the main agent, namely the mixture of the behenic acid imidazoline and the abietic acid imidazoline is obtained.
3) Then, the main agent (the mixture of the behenic acid imidazoline and the abietic acid imidazoline) 28 percent, the dodecylamine 10 percent, the polyoxyethylene alkylphenol ether phosphate 5 percent and the solvent oil 200#57 percent are uniformly mixed according to the mass percentage, so that the oil-soluble corrosion inhibitor for the gathering pipeline pre-film of the embodiment is obtained, and the code is TLM-YM-07.
Example 8
The preparation method of the corrosion inhibitor of the embodiment comprises the following steps:
1) mixing a mixture of two organic acids and diethylenetriamine according to a molar ratio of 1: 1.5 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n; wherein, the two organic acids are behenic acid and erucic acid, and the molar ratio of the behenic acid to the erucic acid is 1: 1;
in the reaction process, water flows out of a condensation pipe at the top of the reaction kettle, and the generated amide of the behenic acid and the amide of the erucic acid;
2) continuously heating to 170 ℃ and 180 ℃, reacting for 1.5h, then continuously heating to 210 ℃ and 220 ℃, preserving the heat for 4h at the temperature, and heating at the speed of not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5mg/kg, and the main agent, namely the mixture of the behenic imidazoline and the erucic imidazoline is obtained.
3) Then, the main agent (the mixture of the behenimidazoline and the erucic acid imidazoline) is 20 percent, the hexadecylamine is 12 percent, the polyoxyethylene alkylphenol ether phosphate ester is 5 percent, and the diesel oil is 63 percent, and the oil-soluble corrosion inhibitor for the gathering pipeline pre-film of the embodiment is obtained, and the code TLM-YM-08 is obtained.
Example 9
The preparation method of the corrosion inhibitor of the embodiment comprises the following steps:
1) mixing a mixture of two organic acids, tetraethylenepentamine according to a molar ratio of 1: 1.5 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n; wherein, the two organic acids are eleostearic acid and abietic acid, and the molar ratio of eleostearic acid to abietic acid is 3: 7;
in the reaction process, water flows out of a condensation pipe at the top of the reaction kettle, and the generated acid amide of eleostearic acid and the acid amide of abietic acid;
2) continuously heating to 170 ℃ and 180 ℃, reacting for 1.5h, then continuously heating to 210 ℃ and 220 ℃, preserving the heat for 4h at the temperature, and heating at the speed of not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5mg/kg, and the main agent, namely the mixture of eleostearic acid imidazoline and abietic acid imidazoline is obtained.
3) Then, 30% of main agent (mixture of eleostearic acid imidazoline and abietic acid imidazoline), 10% of octadecylamine, 10% of polyoxyethylene alkylphenol ether phosphate and 200# 50% of solvent oil are uniformly mixed according to the mass percentage, so that the oil-soluble corrosion inhibitor for gathering and transportation pipeline pre-film of the embodiment is obtained, and the code is TLM-YM-09.
Example 10
The preparation method of the corrosion inhibitor of the embodiment comprises the following steps:
1) mixing a mixture of two organic acids and polyethylene polyamine according to a molar ratio of 1: 1.5 adding the mixture into a reaction kettle, adding a dimethylbenzene water carrying agent (10 percent of the total material amount), heating, stirring, heating to 150 ℃ and 160 ℃, and keeping the temperature for 3 hours, wherein the heating speed is not higher than 20 ℃/10m < 2 > 2 n; wherein, the two organic acids are eleostearic acid and abietic acid, and the molar ratio of eleostearic acid to abietic acid is 1: 3;
in the reaction process, water flows out of a condensation pipe at the top of the reaction kettle, and the generated acid amide of eleostearic acid and the acid amide of abietic acid;
2) continuously heating to 170 ℃ and 180 ℃, reacting for 1.5h, then continuously heating to 210 ℃ and 220 ℃, preserving the heat for 4h at the temperature, and heating at the speed of not higher than 20 ℃/10m < 2 > 2 n;
cooling the reaction system to below 50 ℃, sampling and testing the acid value, wherein the acid value of the reaction system is less than 5mg/kg, and the main agent, namely the mixture of eleostearic acid imidazoline and abietic acid imidazoline is obtained.
3) Then, the oil-soluble corrosion inhibitor for gathering and transportation pipeline pre-film of the embodiment is obtained by uniformly mixing 25 mass percent of a main agent (a mixture of eleostearic acid imidazoline and abietic acid imidazoline), 15 mass percent of dodecylamine, 10 mass percent of polyoxyethylene alkylphenol ether phosphate and 200#50 mass percent of solvent oil, and the code TLM-YM-10 is obtained.
Test examples
In order to test the protection effect of the corrosion inhibitor on the gathering and transportation pipeline, a high-temperature high-pressure test system is adopted to simulate the environment of an oil gathering and transportation system of an oil field to prepare simulated water, and the corrosion inhibitor and diesel oil are mixed according to the contents of an industrial standard SY/T7025-: 1, putting the corrosion sample into the solution, soaking for 3-10s, then removing the sample, fixing the sample on a test container bracket, and preparing for a test.
The test conditions used in the simulation test are shown in table 1, the analysis results of the simulated water sample are shown in table 2, and the used hanging piece sample material is 20G.
Table 3 conditions the corrosion inhibition effect of the oil soluble corrosion inhibitor for pigging and pre-filming of gathering and transportation pipelines in this example was evaluated.
TABLE 1
| Item | Test conditions |
| Temperature, C | 45 |
| Total pressure, MPa | 2 |
| H2S partial pressure, MPa | 0.1 |
| CO2Partial pressure, MPa | 0.5 |
| Test time, day | 7 |
TABLE 2
| NaHCO3 | Na2SO4 | NaCl | CaCl2 | MaCl2 | KCl |
| 1.41 | 1.35 | 378.73 | 125.04 | 11.12 | 6.03 |
TABLE 3
As can be seen from Table 3, the oil-soluble corrosion inhibitor for the pre-film of the gathering pipeline has the corrosion inhibition rate of more than 90 percent and has excellent corrosion prevention effect.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. An oil-soluble corrosion inhibitor for gathering pipeline pre-filming is characterized by comprising the following components in percentage by mass: 20-30% of main agent and 70-80% of compound;
the main agent is composed of a first imidazoline and a second imidazoline, the first imidazoline has a structure of a formula [1], the second imidazoline has a structure of a formula [2],
wherein n is not less than 1 and is a natural number, R1And R2Independently selected from the formula [3]-formula [8]A group represented by, and R1And R2Are different from each other;
"" indicates a bond.
2. An oil-soluble corrosion inhibitor for gathering pipeline pre-filming is characterized by comprising the following components in percentage by mass: 20-30% of main agent and 70-80% of compound; wherein the content of the first and second substances,
the main agent is a product collected when the acid value of a reaction system is less than 5mg/kg after the amidation reaction of organic acid and polyamine substances and the heat preservation at 220 ℃ of 170-; the organic acid comprises two of capric acid, myristic acid, behenic acid, erucic acid, eleostearic acid and abietic acid, the polyamine substance is selected from diethylenetriamine, tetraethylenepentamine or polyethylene polyamine, and the ratio of the sum of the moles of the two organic acids to the moles of the polyamine substance is 1: (1.2-1.5).
3. The corrosion inhibitor of claim 2, wherein during the preparation of said main agent, one of said organic acids is eleostearic acid, and the molar ratio of eleostearic acid to the other of said organic acids is 1 (2-5); or the organic acid comprises two of capric acid, myristic acid, behenic acid, erucic acid and abietic acid, and the molar ratio of the two organic acids is 1: 1.
4. The corrosion inhibitor according to claim 1 or 2, wherein the formulation comprises the following components, based on the total weight of the corrosion inhibitor: 10-15% of alkylamine, 5-19% of phosphate and 45% -65% of solvent.
5. The corrosion inhibitor of claim 4, wherein said alkylamine is selected from the group consisting of dodecylamine, hexadecylamine, and octadecylamine.
6. The corrosion inhibitor of claim 4, wherein said phosphate ester is selected from the group consisting of polyoxyethylene alkylphenol ether phosphate, isotridecanol phosphate and isotridecanol ether phosphate.
7. The corrosion inhibitor according to claim 4, wherein the solvent is selected from one or both of diesel and mineral spirits.
8. The process for preparing the corrosion inhibitor according to any of claims 1 to 7, characterized in that it comprises the following steps:
mixing two organic acids and polyamine substances to carry out amidation reaction, and keeping the temperature of the amidation product system at 170-220 ℃ for more than 1 hour to ensure that the acid value of the reaction system is less than 5mg/kg to obtain the main agent;
at room temperature, mixing the main agent and the compound and uniformly stirring to obtain the corrosion inhibitor;
alternatively, the first and second electrodes may be,
mixing two organic acids with the polyamine substances respectively to perform amidation reaction, keeping the temperature of an amidation product system at 170-220 ℃ for more than 1 hour, ensuring that the acid value of the reaction system is less than 5mg/kg, and mixing the two reaction products to obtain the main agent;
and (3) mixing the main agent and the compound at room temperature, and uniformly stirring to obtain the corrosion inhibitor.
9. The method according to claim 8,
the amidation reaction uses xylene as solvent, the temperature is raised to 150 ℃ and 160 ℃, and the reaction time is maintained for 1-5 hours;
and heating the amidation product system to 170-180 ℃ for continuous reaction for 1-2h, then heating to 210-220 ℃ for heat preservation for 2-5h, and obtaining the main agent when the acid value of the reaction system is less than 5 mg/kg.
10. The method according to claim 9, wherein the temperature rise rate is controlled to be not higher than 20 ℃/10m2 n.
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