CN116770314A - Sterilization corrosion inhibitor for oil field mixed transportation sea pipe and preparation method thereof - Google Patents

Sterilization corrosion inhibitor for oil field mixed transportation sea pipe and preparation method thereof Download PDF

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Publication number
CN116770314A
CN116770314A CN202310513542.8A CN202310513542A CN116770314A CN 116770314 A CN116770314 A CN 116770314A CN 202310513542 A CN202310513542 A CN 202310513542A CN 116770314 A CN116770314 A CN 116770314A
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corrosion inhibitor
aromatic amine
sea pipe
oilfield
sterilization
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陆原
戴俊峰
蓝阳
刘全刚
吴结丰
张国欣
胡廷
刘言霞
邓志强
李羽
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CNOOC Energy Technology and Services Ltd
CNOOC Tianjin Oilfield Chemical Co Ltd
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CNOOC Energy Technology and Services Ltd
CNOOC Tianjin Oilfield Chemical Co Ltd
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    • A01N59/12—Iodine, e.g. iodophors; Compounds thereof
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    • 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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    • 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
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    • 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
    • C23F11/145—Amides; N-substituted amides

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Abstract

The application discloses a sterilization corrosion inhibitor for an oilfield mixed transportation sea pipe and a preparation method thereof, and the preparation method comprises the following steps: stirring and mixing halogenated alkyl hydantoin, aromatic amine, organic amide solvents and iodide, and reacting for 8-12h at 120-150 ℃; cooling, dripping epichlorohydrin, and continuing to react for 8-12h at 15-40 ℃ after dripping; adding mercaptobenzothiazole and potassium hydroxide, vacuumizing and heating to 95-105 ℃, introducing ethylene oxide, continuously reacting for more than 5 hours, heating to 140-160 ℃, continuously reacting until the pressure is reduced to negative pressure, and then cooling to normal temperature; adding low molecular weight polyethylene glycol, 2-dibromo-3-nitrilopropionamide, water, thiourea and thiocyanate, and dissolving to obtain the sterilizing corrosion inhibitor. The bactericidal corrosion inhibitor has good inhibition effect on corrosion and SRB bacteria in a medium, the bactericidal rate is more than 99%, the corrosion inhibition rate is more than 90%, the compatibility is good, the dosage is small, and the bactericidal corrosion inhibition rate is high.

Description

Sterilization corrosion inhibitor for oil field mixed transportation sea pipe and preparation method thereof
Technical Field
The application relates to the technical field of chemical sterilization and corrosion inhibition, in particular to a sterilization and corrosion inhibitor for an oilfield mixed transportation sea pipe and a preparation method thereof.
Background
At present, the mixed transportation sea pipes have serious problems of corrosion and bacterial growth, and huge economic loss is caused. The addition of chemical agents can both effectively and economically control corrosion problems and bacterial growth. However, in order to increase the yield, the method of polymer injection, thermal recovery and the like is usually adopted, and in the processes, an acrylamide polymer is usually required to be added to improve the recovery ratio and an anti-scaling dispersing agent is added to relieve the scale, wherein the acrylamide polymer and the anti-scaling dispersing agent are basically anionic polymers, and are returned along with the produced liquid, so that the effects of a common corrosion inhibitor and a bactericide are greatly reduced in the mixing and conveying process. In order to solve the problems, the preparation of the sterilization corrosion inhibitor with excellent sterilization and corrosion inhibition performances and good compatibility has important significance in well controlling the problems of corrosion and bacterial growth in the mixing and transportation process of the oil field production liquid and the sewage.
Disclosure of Invention
The bactericide can effectively kill the bacteria in the oil field, has the characteristics of good compatibility, small dosage, high sterilization corrosion inhibition rate and the like, and is very suitable for corrosion and bacteria control of the oil field, particularly the offshore oil field, of the mixed transportation sea pipe.
In a first aspect, the application provides a preparation method of a sterilization corrosion inhibitor for an oilfield compound sea pipe, which is realized by adopting the following technical scheme.
The preparation method of the sterilizing corrosion inhibitor for the oil field mixed transportation sea pipe comprises the following steps:
s1, stirring and mixing halogenated alkyl hydantoin, aromatic amine, organic amide solvents and iodide, and reacting for 8-12 hours at 120-150 ℃; the mol ratio of the halogenated alkyl hydantoin to the aromatic amine is (0.9-1.1): 1;
s2, cooling to below 30 ℃, dropwise adding epichlorohydrin, controlling the temperature to be not more than 40 ℃, wherein the molar ratio of the epichlorohydrin to the aromatic amine is (1-1.2): 1; after the dripping is finished, continuing to react for 8 to 12 hours at the temperature of 15 to 40 ℃;
s3, adding mercaptobenzothiazole and potassium hydroxide into the reaction product obtained in the step S2, wherein the molar ratio of the mercaptobenzothiazole to the aromatic amine is (0.1-0.3): 1; vacuumizing and heating to 95-105 ℃, introducing ethylene oxide, and controlling the temperature to be 100-130 ℃ until the molar ratio of the ethylene oxide to the aromatic amine is (8-15): 1; continuously reacting for more than 5 hours, then heating to 140-160 ℃, continuously reacting until the pressure is reduced to negative pressure, and then cooling to normal temperature;
s4, adding low-molecular-weight polyethylene glycol, 2-dibromo-3-nitrilopropionamide (DBNPA), water, thiourea and thiocyanate into the reaction product of the step S3, and dissolving to obtain the sterilizing corrosion inhibitor for the mixed transportation sea pipe.
In the step S1, the dosage of the organic amide solvent is 5-8 times of the mass of the aromatic amine; the organic amide solvent is one or two of N, N-Dimethylformamide (DMF) and N, N-Dimethylacetamide (DMAC).
Further, in the step S1, the iodide is used in an amount of 0.5-1% of the mass of the aromatic amine; the iodide is sodium iodide or potassium iodide.
In step S1, the haloalkylhydantoin is chlorobutyl hydantoin or bromoethyl hydantoin.
In step S1, the aromatic amine is aniline or benzylamine.
Further, in the step S3, the dosage of potassium hydroxide is 0.3% -0.5% of the mass of the aromatic amine.
Further, in step S4, the low molecular weight polyethylene glycol is selected from one or two of polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 600; the amount of the polyethylene glycol with low molecular weight is 3-5 times of the mass of the aromatic amine.
In the step S4, sodium thiocyanate, ammonium thiocyanate or potassium thiocyanate is selected as thiocyanate; the dosage of thiocyanate is 10-20% of the mass of aromatic amine.
Further, in the step S4, the dosage of the 2, 2-dibromo-3-nitrilopropionamide is 10% -20% of the mass of the aromatic amine; the water consumption is 4-6 times of the aromatic amine mass; the consumption of the thiourea is 10-20% of the mass of the aromatic amine.
In a second aspect, the application provides a sterilization corrosion inhibitor for an oilfield compound sea pipe, which is realized by adopting the following technical scheme.
The sterilizing corrosion inhibitor for the oil field mixed transportation sea pipe prepared by the preparation method is provided.
The application has the following beneficial effects.
Aiming at the problem that the performances of the cationic corrosion inhibitor and the bactericide are obviously reduced due to the fact that the medium in the mixed transportation sea pipe contains the anionic polyacrylamide and the anti-scaling dispersant, the application develops a novel sterilization corrosion inhibitor for the mixed transportation sea pipe, which has good inhibition effect on corrosion and SRB bacteria in the medium, has the characteristics of high sterilization rate of more than 99%, high corrosion inhibition rate of more than 90%, good compatibility, small dosage, high sterilization corrosion inhibition rate and the like.
Detailed Description
The present application is further illustrated below with reference to examples.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; materials, reagents and the like used in the following preparation examples and examples are commercially available unless otherwise specified.
Example 1
The preparation method of the sterilizing corrosion inhibitor for the oil field mixed transportation sea pipe comprises the following steps:
step one: 171.56g of chlorobutyl hydantoin (0.9 mol), 93.13g of aniline (1 mol) and 372.52g of DMAC and 372.52g DMF,0.46565g sodium iodide are added into a closed pressure-resistant reaction vessel, stirring is started, the temperature is raised, and the reaction is carried out for 12 hours at 120 ℃;
step two: introducing circulating water to cool to a temperature lower than 30 ℃, slowly dropwise adding 110.04g of epichlorohydrin (1.2 mol), controlling the temperature not to exceed 40 ℃, and continuously reacting for 8 hours at 40 ℃ after the dropwise adding is finished;
step three: 16.73g of mercaptobenzothiazole (0.1 mol) is added, 0.27939g of potassium hydroxide is vacuumized for 5 minutes, then 352.4g of ethylene oxide (8 mol) is slowly introduced after the temperature is raised to 95 ℃, the temperature is controlled to be 100-130 ℃ and is completely introduced, the reaction is continued for more than 5 hours, the temperature is raised to 140 ℃ again, the reaction is continued until the pressure in the kettle is reduced to negative pressure, and then the temperature is reduced to normal temperature;
step four: 279.39g of polyethylene glycol 200 and 9.313g of DBNPA are added into a reaction vessel, uniformly stirred and dissolved, 558.78g of distilled water, 9.313g of thiourea and 18.626g of sodium thiocyanate are added, and uniformly stirred and dissolved, thus obtaining the sterilization corrosion inhibitor A1 for the mixed transportation sea pipe.
Example 2
The preparation method of the sterilizing corrosion inhibitor for the oil field mixed transportation sea pipe comprises the following steps:
step one: 227.73g of bromoethyl hydantoin (1.1 mol), 107.15g of benzylamine (1 mol) and 535.75g DMF,1.07g potassium iodide are added into a closed pressure-resistant reaction vessel, stirring is started, the temperature is raised, and the reaction is carried out for 8 hours at 150 ℃;
step two: introducing circulating water to cool to a temperature lower than 30 ℃, slowly dropwise adding 101.78g of epichlorohydrin (1.1 mol), controlling the temperature not to exceed 40 ℃, and continuously reacting for 12 hours at 15 ℃ after the dropwise adding is finished;
step three: adding 50.19g of mercaptobenzothiazole (0.3 mol), 0.53575g of potassium hydroxide, vacuumizing for 5 minutes, then heating to 100 ℃, slowly introducing 660.75g of ethylene oxide (15 mol), controlling the temperature to be 100-130 ℃, completing the reaction for more than 5 hours, heating to 150 ℃, continuing to react until the pressure in the kettle is reduced to negative pressure, and cooling to normal temperature;
step four: 535.75g of polyethylene glycol 400, 21.43g of DBNPA are added into a reaction vessel, uniformly stirred and dissolved, 428.60g of distilled water, 21.43g of thiourea, 10.715g of sodium thiocyanate are added, and uniformly stirred and dissolved, thus obtaining the sterilization corrosion inhibitor A2 for the mixed transportation sea pipe.
Example 3
The preparation method of the sterilizing corrosion inhibitor for the oil field mixed transportation sea pipe comprises the following steps:
step one: 190.63g of chlorobutyl hydantoin (1 mol), 107.15g of benzylamine (1 mol) and 535.75g of DMF and 107.15g DMAC,8.57g potassium iodide are added into a closed pressure-resistant reaction vessel, stirring is started, the temperature is raised, and the reaction is carried out for 10 hours at 140 ℃;
step two: cooling to a temperature lower than 30 ℃ by circulating water, slowly dropwise adding 92.53g of epichlorohydrin (1 mol), controlling the temperature not to exceed 40 ℃, and continuing to react for 10 hours at 20 ℃ after the dropwise adding is finished;
step three: adding 33.45g of mercaptobenzothiazole (0.2 mol), 0.4286g of potassium hydroxide, vacuumizing for 5 minutes, then heating to 105 ℃, slowly introducing 440.50g of ethylene oxide (10 mol), controlling the temperature to be 100-130 ℃, completing the reaction for more than 5 hours, heating to 160 ℃, continuing the reaction until the pressure in the kettle is reduced to negative pressure, and cooling to normal temperature;
step four: 321.45g of polyethylene glycol 200 and 214.30g of polyethylene glycol 600, 16.07g of DBNPA are added into a reaction vessel, uniformly stirred and dissolved, 535.75g of distilled water, 16.07g of thiourea and 16.07g of sodium thiocyanate are added, and uniformly stirred and dissolved, thus obtaining the sterilizing corrosion inhibitor A3 for the mixed transportation sea pipe.
Example 4
The preparation method of the sterilizing corrosion inhibitor for the oil field mixed transportation sea pipe comprises the following steps:
step one: 207.03g of bromoethyl hydantoin (1 mol), 93.13g of aniline (1 mol), 465.65g of DMF and 186.26g of DMAC and 9g of potassium iodide are added into a closed pressure-resistant reaction vessel, stirring is started, the temperature is raised, and the reaction is carried out for 11 hours at 130 ℃;
step two: introducing circulating water to cool to a temperature lower than 30 ℃, slowly dropwise adding 101.78g of epichlorohydrin (1.1 mol), controlling the temperature not to exceed 40 ℃, and continuing to react for 9 hours at the temperature of 30 ℃ after the dropwise adding is finished;
step three: adding 33.45g of mercaptobenzothiazole (0.2 mol), 0.40g of potassium hydroxide, vacuumizing for 5 minutes, then heating to 100 ℃, slowly introducing 528.60g of ethylene oxide (12 mol), controlling the temperature to be 100-130 ℃, completing the reaction for more than 5 hours, heating to 150 ℃, continuing the reaction until the pressure in the kettle is reduced to negative pressure, and cooling to normal temperature;
step four: 190.00g of polyethylene glycol 200 and 180.00g of polyethylene glycol 400 and 15.00g of DBNPA are added into a reaction vessel, uniformly stirred and dissolved, 535.75g of distilled water, 10.00g of thiourea and 18.00g of sodium thiocyanate are added, uniformly stirred and dissolved, and the sterilizing corrosion inhibitor A4 for the mixed transportation sea pipe is prepared.
Application example 1
Experimental raw materials: the content of blank SRB bacteria in the polymer-containing produced liquid of some offshore oil field is 1.2 multiplied by 10 3 personal/mL
Evaluation mode: dilution method for eliminating trace
Experimental temperature: 80 DEG C
Test time: 168h
Concentration of the agent: 30mg/L
The test results were as follows:
TABLE 1 Sterilization test results
Application example 2
Experimental raw materials: production sewage filled with anionic polymer antiscaling agent in offshore oil field with blank SRB bacteria content of 0.9X10 6 personal/mL
Evaluation mode: dilution method for eliminating trace
Experimental temperature: 60 DEG C
Test time: 168h
Concentration of the agent: 60mg/L
The test results were as follows:
TABLE 2 Sterilization test results
From the detection data, the application has good inhibition effect on SRB bacteria in the production sewage of some offshore oil fields filled with the anionic polymer scale inhibitor, and the sterilization rate is more than 99%, obviously due to the common oilfield bactericides.
Application example 3
Experimental medium: the method for evaluating the polymer-containing produced fluid of the offshore oil field comprises the following steps: laboratory 3 liter Hastelloy steel kettle dynamic corrosion experiment materials: 20# steel
Experimental temperature: 80 DEG C
Medium flow rate: 1.0m/s
Experimental gas phase composition: 0.25MPa CO 2 +0.7MPaN 2
Test time: indoor experiment for 72 hours
Concentration of the agent: 30mg/L
The test results were as follows:
TABLE 3 results of indoor dynamic Corrosion test
Application example 4
Experimental medium: production sewage filled with anionic polymer scale inhibitor for offshore oil field
Evaluation mode: dynamic corrosion experiment of indoor 3 liter hastelloy steel kettle
Experimental materials: q235 steel
Experimental temperature: 60 DEG C
Medium flow rate: 1.2m/s
Experimental gas phase composition: 0.20MPa CO 2 +0.50MPaN 2
Test time: indoor experiment for 72 hours
Concentration of the agent: 20mg/L
The test results were as follows:
TABLE 4 indoor dynamic Corrosion results
From the detection data, compared with the conventional corrosion inhibitors such as various organic phosphines, heterocyclic compounds and the like, the bactericidal corrosion inhibitor has higher efficient corrosion inhibition effect on the production sewage containing polymer produced liquid and the anionic polymer antiscaling agent in the oil field.
The embodiments of the present application are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in this way, therefore: all equivalent changes in structure, shape and principle of the application should be covered in the scope of protection of the application.

Claims (10)

1. A preparation method of a sterilization corrosion inhibitor for an oilfield mixed transportation sea pipe is characterized by comprising the following steps: the method comprises the following steps:
s1, stirring and mixing halogenated alkyl hydantoin, aromatic amine, organic amide solvents and iodide, and reacting for 8-12 hours at 120-150 ℃; the mol ratio of the halogenated alkyl hydantoin to the aromatic amine is (0.9-1.1): 1;
s2, cooling to below 30 ℃, dropwise adding epichlorohydrin, controlling the temperature to be not more than 40 ℃, wherein the molar ratio of the epichlorohydrin to the aromatic amine is (1-1.2): 1; after the dripping is finished, continuing to react for 8 to 12 hours at the temperature of 15 to 40 ℃;
s3, adding mercaptobenzothiazole and potassium hydroxide into the reaction product obtained in the step S2, wherein the molar ratio of the mercaptobenzothiazole to the aromatic amine is (0.1-0.3): 1; vacuumizing and heating to 95-105 ℃, introducing ethylene oxide, and controlling the temperature to be 100-130 ℃ until the molar ratio of the ethylene oxide to the aromatic amine is (8-15): 1; continuously reacting for more than 5 hours, then heating to 140-160 ℃, continuously reacting until the pressure is reduced to negative pressure, and then cooling to normal temperature;
s4, adding low-molecular-weight polyethylene glycol, 2-dibromo-3-nitrilopropionamide, water, thiourea and thiocyanate into the reaction product of the step S3, and dissolving to obtain the sterilizing corrosion inhibitor for the mixed transportation sea pipe.
2. The method for preparing the sterilization corrosion inhibitor for the oilfield compound sea pipe, which is disclosed in claim 1, is characterized in that: in the step S1, the dosage of the organic amide solvent is 5-8 times of the mass of the aromatic amine; the organic amide solvent is one or two of N, N-dimethylformamide and N, N-dimethylacetamide.
3. The method for preparing the sterilization corrosion inhibitor for the oilfield compound sea pipe, which is disclosed in claim 1, is characterized in that: in the step S1, the iodide dosage is 0.5-1% of the aromatic amine mass; the iodide is sodium iodide or potassium iodide.
4. The method for preparing the sterilization corrosion inhibitor for the oilfield compound sea pipe, which is disclosed in claim 1, is characterized in that: in the step S1, the halogenated alkyl hydantoin is chlorobutyl hydantoin or bromoethyl hydantoin.
5. The method for preparing the sterilization corrosion inhibitor for the oilfield compound sea pipe, which is disclosed in claim 1, is characterized in that: in the step S1, the aromatic amine is aniline or benzylamine.
6. The method for preparing the sterilization corrosion inhibitor for the oilfield compound sea pipe, which is disclosed in claim 1, is characterized in that: in the step S3, the dosage of potassium hydroxide is 0.3-0.5% of the mass of the aromatic amine.
7. The method for preparing the sterilization corrosion inhibitor for the oilfield compound sea pipe, which is disclosed in claim 1, is characterized in that: in the step S4, the polyethylene glycol with low molecular weight is selected from one or two of polyethylene glycol 200, polyethylene glycol 400 and polyethylene glycol 600; the amount of the polyethylene glycol with low molecular weight is 3-5 times of the mass of the aromatic amine.
8. The method for preparing the sterilization corrosion inhibitor for the oilfield compound sea pipe, which is disclosed in claim 1, is characterized in that: in the step S4, sodium thiocyanate, ammonium thiocyanate or potassium thiocyanate is selected as thiocyanate; the dosage of thiocyanate is 10-20% of the mass of aromatic amine.
9. The method for preparing the sterilization corrosion inhibitor for the oilfield compound sea pipe, which is disclosed in claim 1, is characterized in that: in the step S4, the dosage of the 2, 2-dibromo-3-nitrilopropionamide is 10-20% of the mass of the aromatic amine; the water consumption is 4-6 times of the aromatic amine mass; the consumption of the thiourea is 10-20% of the mass of the aromatic amine.
10. A sterilizing corrosion inhibitor for an oilfield compound sea pipe prepared by the preparation method of any one of claims 1 to 9.
CN202310513542.8A 2023-05-09 2023-05-09 Sterilization corrosion inhibitor for oil field mixed transportation sea pipe and preparation method thereof Pending CN116770314A (en)

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