CN112778992A - Corrosion inhibitor for annular protection liquid and preparation method and application thereof - Google Patents
Corrosion inhibitor for annular protection liquid and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a corrosion inhibitor for an annular space protection liquid, a preparation method and application thereof, wherein the preparation method comprises the steps of mixing alcohol amine and phosphorus pentoxide, and reacting at 60-100 ℃ for 1-3h to obtain organic amine ester A; uniformly mixing the organic amine ester A and the organic acid, stirring and reacting at 75-110 ℃ for 1-3h to obtain organic amine ester B; mixing the organic amine lipid B and sorbitol uniformly, stirring and reacting at 80-120 ℃ for 1-3h to obtain organic amine lipid C; and (3) mixing and stirring the organic amine ester C, the imidazoline quaternary ammonium salt, the ethanol and the thiourea uniformly to obtain the corrosion inhibitor for the annular space protection liquid. The corrosion inhibitor for the annular space protection liquid is an organic amine ester corrosion inhibitor, and has the characteristics of quick film forming, long period of metal protection material, low corrosion rate, stable property, good compatibility, low production cost, simple process, universal applicability and the like.
Description
Technical Field
The invention relates to the technical field of oil-gas-water treatment, in particular to a corrosion inhibitor for an environment protection liquid, and a preparation method and application thereof.
Background
After oil field development generally enters the middle and later stages of water injection development, the water content of produced liquid is increased year by year, the corrosion and damage problems of oil pipes and casings of oil and gas wells and water injection wells are increasingly serious, so that the oil and water wells are frequently repaired or even scrapped, and the economic loss is huge.
The annular protection fluid is filled between an oil pipe and an oil layer casing pipe and has the following functions: (1) reducing the oil gas pressure borne by a casing head or a packer; meanwhile, a certain sealing effect is achieved, and the packer is prevented from being punctured and leaked; (2) the pressure difference between the oil pipe and the annulus is reduced; (3) inhibit the corrosion and scale inhibition tendency of oil pipes and casings, namely have corrosion resistance and stability.
The annular protection liquid is divided into water-based annular protection liquid and oil-based annular protection liquid, and the oil-based annular protection liquid is more corrosion-resistant and better in thermal stability than the water-based annular protection liquid. However, when the high salinity brine is encountered, problems such as solid phase deposition and the like can occur. Meanwhile, the oil-based annular protection fluid cannot be widely popularized and applied due to factors such as high unit cost and the like; the water-based annular protection fluid is low in price but is greatly influenced by factors such as water quality and the like, the produced fluid of the oil well contains a large amount of water and has high mineralization degree, and crude oilAssociated gas containing CO2、H2The problems of corrosion and scaling frequently occur due to various conditions such as a great amount of breeding and propagation of corrosive bacteria SRB in corrosive gases such as S.
The corrosion of the well bore to a certain degree can bring great harm to the production of the oil field, and the main points are as follows: a. increasing the natural degressive property of the oil field; b. the water injection well pattern is incomplete, the water driving degree is reduced, and the oil field recovery ratio is influenced; c. the production increasing measures and the well repairing difficulty are increased, and the operation cost is increased; d. resulting in poor water flooding development effect and affecting the oil extraction speed of the oil field.
More than 90% of foreign oil fields are mainly prevented in the initial development stage, research on corrosion influencing factors is developed, the corrosion influencing factors are researched, and corrosion protection measures are taken in a targeted manner. With respect to corrosion control issues, the following three types of corrosion protection techniques can generally be considered: corrosion resistant materials, undercoats, and corrosion inhibitors. The method has good economic and social benefits. Practical experience at home and abroad shows that: among the above 3 methods, the corrosion inhibitor is the most economical, reliable and flexible corrosion control method, and is most widely used in oil and gas fields. At present, a plurality of land oil fields in China also use foreign methods for carrying out corrosion prevention research on mineshafts, and a great deal of work is carried out in recent years, wherein the annular space protection liquid is the most advantageous one.
Aiming at the corrosion condition of the ring sleeve, the purpose of controlling corrosion is achieved by adding components of a corrosion inhibitor into the annular protection liquid in each large oil field. At present, the corrosion inhibitors applied to oil and gas well casings are inorganic passivation corrosion inhibitors (chromate type), oxygen removal corrosion inhibitors (sodium nitrite type), organic amine corrosion inhibitors such as primary amine, secondary amine, ethylenediamine polyamine, phthalein amine, imidazoline and amine compounds.
Disclosure of Invention
The corrosion inhibitor for the annular space protection liquid is an organic amine ester corrosion inhibitor and has the characteristics of quick film forming, long period of metal material protection period, low corrosion rate, stable property, good compatibility, low production cost, simple process, universal applicability and the like.
The purpose of the invention is realized by the following technical scheme.
The corrosion inhibitor for the annular space protection liquid and the preparation method thereof are carried out according to the following steps:
step 1, mixing alcohol amine and phosphorus pentoxide, and reacting at 60-100 ℃ for 1-3h to obtain organic amine ester A, wherein the molar ratio of the alcohol amine to the phosphorus pentoxide is (2-4) to 1, and the alcohol amine is ethanolamine, diethanolamine or triethanolamine;
step 2, uniformly mixing the organic amine ester A prepared in the step 1 with an organic acid, stirring and reacting at 75-110 ℃ for 1-3h to obtain an organic amine ester B, wherein the molar ratio of the organic amine ester A to the organic acid is (1-5): 1, adopting benzoic acid or maleic acid as the organic acid;
and 3, uniformly mixing the organic amine lipid B prepared in the step 2 with sorbitol, stirring and reacting at 80-120 ℃ for 1-3h to obtain an organic amine lipid C, wherein the molar ratio of the organic amine lipid B to the sorbitol is (1-3): 1;
and 4, mixing and stirring the organic amine ester C prepared in the step 3, imidazoline quaternary ammonium salt, ethanol and thiourea uniformly to obtain the corrosion inhibitor for the annular space protection liquid, wherein the imidazoline quaternary ammonium salt is oleic imidazoline benzyl chloride quaternary ammonium salt or naphthenic imidazoline benzyl chloride quaternary ammonium salt, and the mass ratio of the organic amine ester C to the imidazoline quaternary ammonium salt to the ethanol to the thiourea is (6-8): (1-3): (3-5): (1-2).
In the step 1, the molar ratio of the alcohol amine to the phosphorus pentoxide is 3:1, and the alcohol amine and the phosphorus pentoxide are mixed and react for 2 hours at the temperature of 70-90 ℃.
In step 2, the molar ratio of the organic amine ester A to the organic acid is (2-4):1, uniformly mixing organic amine ester A and organic acid, and stirring and reacting for 2 hours at 80-100 ℃.
In step 3, the mole ratio of the organic amine lipid B to the sorbitol is (1-2): 1, uniformly mixing organic amine ester B and sorbitol, and stirring and reacting for 2 hours at 90-110 ℃.
In the step 4, the mass ratio of the organic amine ester C, the imidazoline quaternary ammonium salt, the ethanol and the thiourea is 7: 2: 4: 1.
the invention has the beneficial effects that: the corrosion inhibitor for the annular protection liquid has the advantages of being fast in film forming property and surface activity, capable of forming a film rapidly, capable of isolating contact between water quality and metal pipeline materials through coordination bonds formed by lone-pair electrons of nitrogen atoms and empty orbits of iron elements, and achieving a good corrosion inhibition effect.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
The oleic imidazoline benzyl chloride quaternary ammonium salt is purchased from Zhonghai oil Tianjin chemical research design institute, Inc.; naphthenic acid imidazoline benzyl chloride quaternary ammonium salt is purchased from the chemical research and design institute of Tianjin, Inc. of Zhonghai oil.
Example 1
(1) Firstly, mixing 18.3g of ethanolamine and 14.2g of phosphorus pentoxide (wherein the mass ratio of the triethanolamine to the phosphorus pentoxide is 3:1), heating to 90 ℃, and stirring for 2 hours to obtain organic amine ester A1;
(2) mixing the organic amine lipid A1 obtained in the step (1) with 18.4g of benzoic acid (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid A1 to the benzoic acid is 2:1) uniformly, heating to 100 ℃, stirring for 2h, and reacting to obtain organic amine lipid B1;
(3) mixing the organic amine lipid B1 obtained in the step (2) with 54.9g of sorbitol (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid B1 to the sorbitol is 1:1), heating to 110 ℃, stirring for 2 hours, and reacting to obtain organic amine lipid C1;
(4) the mass ratio of the organic amine ester C to the imidazoline quaternary ammonium salt to the ethanol to the thiourea is 7: 2: 4:1, stirring uniformly to obtain the corrosion inhibitor.
Example 2
(1) Firstly, mixing 31.5g of diethanolamine and 14.2g of phosphorus pentoxide (wherein the mass ratio of the diethanolamine to the phosphorus pentoxide is 3:1), heating to 70 ℃, and stirring for 2 hours to obtain organic amine ester A2;
(2) mixing the organic amine lipid A2 obtained in the step (1) with 12.3g of benzoic acid (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid A2 to the benzoic acid is 3:1) uniformly, heating to 80 ℃, stirring for 2h, and reacting to obtain organic amine lipid B2;
(3) mixing the organic amine lipid B2 obtained in the step (2) with 27.5g of sorbitol (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid B2 to the sorbitol is 2:1), heating to 90 ℃, stirring for 2 hours, and reacting to obtain organic amine lipid C2;
(4) the mass ratio of the organic amine ester C to the imidazoline quaternary ammonium salt to the ethanol to the thiourea is 7: 2: 4:1, stirring uniformly to obtain the corrosion inhibitor.
Example 3
(1) Firstly, mixing 44.8g of triethanolamine and 14.2g of phosphorus pentoxide (wherein the mass ratio of the triethanolamine to the phosphorus pentoxide is 3:1), heating to 80 ℃, and stirring for 2 hours to obtain organic amine ester A3;
(2) mixing the organic amine lipid A3 obtained in the step (1) with 9.2g of benzoic acid (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid A3 to the benzoic acid is 4:1) uniformly, heating to 90 ℃, stirring for 2h, and reacting to obtain organic amine lipid B3;
(3) mixing the organic amine lipid B3 obtained in the step (2) with 36.6g of sorbitol (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid B3 to the sorbitol is 3:2), heating to 100 ℃, stirring for 2 hours, and reacting to obtain organic amine lipid C3;
(4) the mass ratio of the organic amine ester C to the imidazoline quaternary ammonium salt to the ethanol to the thiourea is 7: 2: 4:1, stirring uniformly to obtain the corrosion inhibitor.
Example 4
(1) Firstly, mixing 18.3g of ethanolamine and 14.2g of phosphorus pentoxide (wherein the mass ratio of the triethanolamine to the phosphorus pentoxide is 3:1), heating to 70 ℃, and stirring for 2 hours to obtain organic amine ester A4;
(2) mixing the organic amine lipid A4 obtained in the step (1) with 17.5g of maleic acid (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid A4 to the maleic acid is 2:1) uniformly, heating to 80 ℃, stirring for 2h, and reacting to obtain organic amine lipid B4;
(3) mixing the organic amine lipid B4 obtained in the step (2) with 54.9g of sorbitol (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid B4 to the sorbitol is 1:1), heating to 90 ℃, stirring for 2 hours, and reacting to obtain organic amine lipid C4;
(4) the mass ratio of the organic amine ester C to the imidazoline quaternary ammonium salt to the ethanol to the thiourea is 7: 2: 4:1, stirring uniformly to obtain the corrosion inhibitor.
Example 5
(1) Firstly, mixing 31.5g of diethanolamine and 14.2g of phosphorus pentoxide (wherein the mass ratio of the diethanolamine to the phosphorus pentoxide is 3:1), heating to 80 ℃, and stirring for 2 hours to obtain organic amine ester A5;
(2) mixing the organic amine lipid A5 obtained in the step (1) with 11.7g of maleic acid (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid A5 to the maleic acid is 3:1) uniformly, heating to 90 ℃, stirring for 2h, and reacting to obtain organic amine lipid B5;
(3) mixing the organic amine lipid B5 obtained in the step (2) with 27.5g of sorbitol (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid B5 to the sorbitol is 2:1), heating to 90 ℃, stirring for 2 hours, and reacting to obtain organic amine lipid C5;
(4) the mass ratio of the organic amine ester C to the imidazoline quaternary ammonium salt to the ethanol to the thiourea is 7: 2: 4:1, stirring uniformly to obtain the corrosion inhibitor.
Example 6
(1) Firstly, mixing 44.8g of triethanolamine and 14.2g of phosphorus pentoxide (wherein the mass ratio of the triethanolamine to the phosphorus pentoxide is 3:1), heating to 90 ℃, and stirring for 2 hours to obtain organic amine ester A6;
(2) mixing the organic amine lipid A6 obtained in the step (1) with 8.7g of maleic acid (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid A6 to the maleic acid is 4:1) uniformly, heating to 90 ℃, stirring for 2h, and reacting to obtain organic amine lipid B6;
(3) mixing the organic amine lipid B6 obtained in the step (2) with 36.6g of sorbitol (analytically pure, with the mass concentration of 99.5%) (wherein the mass ratio of the organic amine lipid B6 to the sorbitol is 3:2), heating to 100 ℃, stirring for 2 hours, and reacting to obtain organic amine lipid C6;
(4) the mass ratio of the organic amine ester C to the imidazoline quaternary ammonium salt to the ethanol to the thiourea is 7: 2: 4:1, stirring uniformly to obtain the corrosion inhibitor.
Evaluation experiment I
Experiment raw materials: water source well water of offshore oil field (degree of mineralization 50000mg/L)
Experiment temperature: 40 deg.C
The concentration of the medicament: 1 percent of
Evaluation criteria: SY/T5273 evaluation method for corrosion inhibitor performance of oilfield produced water
The evaluation method comprises the following steps: the method is carried out under the condition that the water body is not deoxidized and dissolved oxygen is directly reserved, a corrosion inhibitor sample with the mass concentration of 1% is added into 100mL of water sample, a 20# steel metal hanging piece is hung, and standing is carried out for fifteen days.
TABLE 1 aerobic Corrosion test data
And (3) removing oxygen in the water body in vacuum, and then introducing carbon dioxide and hydrogen sulfide, and then evaluating the result of the corrosion inhibitor, wherein the water body simulates the corrosion under the condition of dissolved carbon dioxide and hydrogen sulfide. Adding a corrosion inhibitor sample with the mass concentration of 1% into 2000mL of water sample, hanging a 20# steel metal hanging piece, and standing for seven days.
TABLE 2 Corrosion test data under oxygen-free carbon dioxide conditions
Evaluation experiment two
Experiment raw materials: production sewage of certain oil field (degree of mineralization 150000mg/L)
Experiment temperature: 40 deg.C
The concentration of the medicament: 1 percent of
Evaluation criteria: SY/T5273 evaluation method for corrosion inhibitor performance of oilfield produced water
The evaluation method comprises the following steps: the method is carried out under the condition that the water body is not deoxidized and dissolved oxygen is directly reserved, a corrosion inhibitor sample with the mass concentration of 1% is added into 100mL of water sample, a 20# steel metal hanging piece is hung, and standing is carried out for fifteen days.
TABLE 3 aerobic Corrosion test data
And (3) removing oxygen from the water body in vacuum, introducing carbon dioxide and hydrogen sulfide, removing oxygen, and then evaluating the result of the corrosion inhibitor, wherein the water body simulates the corrosion under the conditions of soluble carbon dioxide and hydrogen sulfide. Adding a corrosion inhibitor sample with the mass concentration of 1% into 2000mL of water sample, hanging a 20# steel metal hanging piece, and standing for seven days.
TABLE 4 Corrosion test data under oxygen-free carbon dioxide conditions
Evaluation experiment III
Experiment raw materials: water source well water of offshore oil field (mineralization 1000mg/L)
Experiment temperature: 40 deg.C
The concentration of the medicament: 1 percent of
Evaluation criteria: SY/T5273 evaluation method for corrosion inhibitor performance of oilfield produced water
The evaluation method comprises the following steps: the method is carried out under the condition that the water body is not deoxidized and dissolved oxygen is directly reserved, a corrosion inhibitor sample with the mass concentration of 1% is added into 100mL of water sample, a 20# steel metal hanging piece is hung, and standing is carried out for fifteen days.
TABLE 5 aerobic Corrosion test data
And (3) removing oxygen in the water body in vacuum, and then introducing carbon dioxide and hydrogen sulfide, and then evaluating the result of the corrosion inhibitor, wherein the water body simulates the corrosion under the condition of dissolved carbon dioxide and hydrogen sulfide. Adding a corrosion inhibitor sample with the mass concentration of 1% into 2000mL of water sample, hanging a 20# steel metal hanging piece, and standing for seven days.
TABLE 6 Corrosion test data under oxygen-free carbon dioxide conditions
Therefore, the corrosion inhibitor for the annular protection fluid has the characteristics of small dosage, high corrosion inhibition rate and good compatibility on an annular protection fluid system consisting of offshore oil field water source well water and production water.
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. The corrosion inhibitor for the annular space protection liquid is characterized in that: the method comprises the following steps:
step 1, mixing alcohol amine and phosphorus pentoxide, and reacting at 60-100 ℃ for 1-3h to obtain organic amine ester A, wherein the molar ratio of the alcohol amine to the phosphorus pentoxide is (2-4) to 1, and the alcohol amine is ethanolamine, diethanolamine or triethanolamine;
step 2, uniformly mixing the organic amine ester A prepared in the step 1 with an organic acid, stirring and reacting at 75-110 ℃ for 1-3h to obtain an organic amine ester B, wherein the molar ratio of the organic amine ester A to the organic acid is (1-5): 1, adopting benzoic acid or maleic acid as the organic acid;
and 3, uniformly mixing the organic amine lipid B prepared in the step 2 with sorbitol, stirring and reacting at 80-120 ℃ for 1-3h to obtain an organic amine lipid C, wherein the molar ratio of the organic amine lipid B to the sorbitol is (1-3): 1;
and 4, mixing and stirring the organic amine ester C prepared in the step 3, imidazoline quaternary ammonium salt, ethanol and thiourea uniformly to obtain the corrosion inhibitor for the annular space protection liquid, wherein the imidazoline quaternary ammonium salt is oleic imidazoline benzyl chloride quaternary ammonium salt or naphthenic imidazoline benzyl chloride quaternary ammonium salt, and the mass ratio of the organic amine ester C to the imidazoline quaternary ammonium salt to the ethanol to the thiourea is (6-8): (1-3): (3-5): (1-2).
2. The corrosion inhibitor for an annulus protection fluid of claim 1, wherein: in the step 1, the molar ratio of the alcohol amine to the phosphorus pentoxide is 3:1, and the alcohol amine and the phosphorus pentoxide are mixed and react for 2 hours at the temperature of 70-90 ℃.
3. The corrosion inhibitor for an annulus protection fluid of claim 1, wherein: in step 2, the molar ratio of the organic amine ester A to the organic acid is (2-4):1, uniformly mixing organic amine ester A and organic acid, and stirring and reacting for 2 hours at 80-100 ℃.
4. The corrosion inhibitor for an annulus protection fluid of claim 1, wherein: in step 3, the mole ratio of the organic amine lipid B to the sorbitol is (1-2): 1, uniformly mixing organic amine ester B and sorbitol, and stirring and reacting for 2 hours at 90-110 ℃.
5. The corrosion inhibitor for an annulus protection fluid of claim 1, wherein: in the step 4, the mass ratio of the organic amine ester C, the imidazoline quaternary ammonium salt, the ethanol and the thiourea is 7: 2: 4: 1.
6. the preparation method of the corrosion inhibitor for the annular space protection liquid is characterized by comprising the following steps: the method comprises the following steps:
step 1, mixing alcohol amine and phosphorus pentoxide, and reacting at 60-100 ℃ for 1-3h to obtain organic amine ester A, wherein the molar ratio of the alcohol amine to the phosphorus pentoxide is (2-4) to 1, and the alcohol amine is ethanolamine, diethanolamine or triethanolamine;
step 2, uniformly mixing the organic amine ester A prepared in the step 1 with an organic acid, stirring and reacting at 75-110 ℃ for 1-3h to obtain an organic amine ester B, wherein the molar ratio of the organic amine ester A to the organic acid is (1-5): 1, adopting benzoic acid or maleic acid as the organic acid;
and 3, uniformly mixing the organic amine lipid B prepared in the step 2 with sorbitol, stirring and reacting at 80-120 ℃ for 1-3h to obtain an organic amine lipid C, wherein the molar ratio of the organic amine lipid B to the sorbitol is (1-3): 1;
and 4, mixing and stirring the organic amine ester C prepared in the step 3, imidazoline quaternary ammonium salt, ethanol and thiourea uniformly to obtain the corrosion inhibitor for the annular space protection liquid, wherein the imidazoline quaternary ammonium salt is oleic imidazoline benzyl chloride quaternary ammonium salt or naphthenic imidazoline benzyl chloride quaternary ammonium salt, and the mass ratio of the organic amine ester C to the imidazoline quaternary ammonium salt to the ethanol to the thiourea is (6-8): (1-3): (3-5): (1-2).
7. The method for preparing the corrosion inhibitor for the annular space protection fluid according to claim 6, wherein the method comprises the following steps: in the step 1, the molar ratio of the alcohol amine to the phosphorus pentoxide is 3:1, and the alcohol amine and the phosphorus pentoxide are mixed and react for 2 hours at the temperature of 70-90 ℃.
8. The method for preparing the corrosion inhibitor for the annular space protection fluid according to claim 6, wherein the method comprises the following steps: in step 2, the molar ratio of the organic amine ester A to the organic acid is (2-4):1, uniformly mixing organic amine ester A and organic acid, and stirring and reacting for 2 hours at 80-100 ℃.
9. The method for preparing the corrosion inhibitor for the annular space protection fluid according to claim 6, wherein the method comprises the following steps: in step 3, the mole ratio of the organic amine lipid B to the sorbitol is (1-2): 1, uniformly mixing organic amine ester B and sorbitol, and stirring and reacting for 2 hours at 90-110 ℃; in the step 4, the mass ratio of the organic amine ester C, the imidazoline quaternary ammonium salt, the ethanol and the thiourea is 7: 2: 4: 1.
10. use of a corrosion inhibitor for an annulus protection fluid according to any one of claims 1 to 5 for well annulus protection of highly mineralized brine, characterized in that: under the salinity of the salt water of 1000-150000mg/L, the aerobic corrosion inhibition rate of the corrosion inhibitor for the annular protection liquid is 82-89%, and the anaerobic corrosion inhibition rate of the corrosion inhibitor for the annular protection liquid is 82-94%.
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