CN114958325B - High-temperature-resistant corrosion inhibitor, preparation method and application thereof in shaft corrosion prevention - Google Patents
High-temperature-resistant corrosion inhibitor, preparation method and application thereof in shaft corrosion prevention Download PDFInfo
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- C07D251/02—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings
- C07D251/12—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members
- C07D251/26—Heterocyclic compounds containing 1,3,5-triazine rings not condensed with other rings having three double bonds between ring members or between ring members and non-ring members with only hetero atoms directly attached to ring carbon atoms
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Abstract
The invention discloses a high-temperature-resistant corrosion inhibitor, a preparation method and application thereof in shaft corrosion prevention. The preparation method comprises the steps of S1, mixing trichlorotriazine with an organic solvent 1, refluxing, adding dimethylamine, carrying out reflux reaction, cooling, and concentrating under reduced pressure to obtain A; s2, mixing chlorobutyric acid and dicyclohexylcarbodiimide, adding dopamine into dichloromethane serving as a solvent under the stirring condition, reacting, precipitating with diethyl ether, and performing suction filtration to obtain B; and S3, dissolving the B obtained in the step S2 in the organic solvent 2, dropwise adding the A obtained in the step S1 under the reflux condition, continuing to reflux after the dropwise adding is finished, cooling, concentrating under reduced pressure, precipitating with diethyl ether, and washing to obtain the organic solvent. The high-temperature resistant corrosion inhibitor of the invention has the mineralization degree higher than 20000mg/L and is rich in CO at the temperature higher than 150 DEG C 2 And H 2 The S has better anti-corrosion effect under the environment condition.
Description
Technical Field
The invention relates to the technical field of metal corrosion prevention, in particular to a high-temperature-resistant corrosion inhibitor, a preparation method and application thereof in shaft corrosion prevention.
Background
The problem of metal corrosion is prevalent. The steel in the petroleum industry is used in a large quantity, and the environment where the oil field is located is complex, so that the oil gas well and even the whole oil gas gathering and transportation production, storage and transportation system have corrosion with different degrees. The corrosion damage causes production accidents, causes economic loss, seriously affects the normal production of the oil-gas field and restricts the improvement of economic benefit. Therefore, oil and gas field corrosion and protection work has been one of the important tasks of the petroleum industry.
The corrosion inhibitor is the most effective and cheap method in metal corrosion protection, and is widely applied in the petroleum and natural gas exploitation and gathering process. The corrosion inhibitor is adsorbed on the metal surface through physical adsorption or chemical adsorption of polar groups on molecules, so that on one hand, the energy state of the metal surface tends to be stable, the activation energy of corrosion reaction is improved, and the corrosion speed is reduced; on the other hand, a layer of hydrophobic protective film can be formed on the surface of the metal to prevent corrosion.
CN102730890a discloses a gas phase corrosion inhibitor for carbon dioxide-containing natural gas. The composition comprises the following components in percentage by weight: 10-20% of N-methyldiethanolamine, 1-3% of sec-octanol polyoxyethylene ether, 3-10% of benzotriazole, 4-15% of 5, 7-dinitrogen-8-hydroxyquinoline and 52-82% of absolute ethyl alcohol.
CN108048065a discloses a corrosion inhibitor for oil and gas wells, its preparation method and application, the corrosion inhibitor for oil and gas wells comprises, by weight percentage, 100%: 40% -60% of imidazoline derivative, 8% -40% of organic phosphonate, 30% -50% of dispersing agent and 2% -15% of surfactant. The oil-gas well corrosion inhibitor has the advantages of high temperature resistance, stable performance and excellent corrosion inhibition effect, is suitable for crude oil media in oil wells and gas media in gas wells, is also suitable for water media of water injection wells in oil fields, and has a good corrosion resistance effect.
With the increasing development of exploration and development technology, deep-ultra-deep oil gas development is an important successor field of oil gas resources. An important difficulty facing deep-ultra-deep oil and gas development is that the reservoir temperature and water mineralization degree are higher and higher along with the increase of the exploitation depth, so that the well bore is severely corroded. The prior corrosion inhibitor suitable for shaft corrosion prevention under high temperature condition is few, especially at the temperature higher than 150 ℃, has high mineralization degree and is rich in CO 2 And H 2 The underground corrosion inhibitor in the S environment has not been reported yet.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-temperature-resistant corrosion inhibitor, a preparation method and application thereof in shaft corrosion prevention, wherein triazine ring, benzene ring and hydroxyl are introduced into the corrosion inhibitor molecule, so that the binding capacity and the number of binding sites of the molecule and the metal surface are increased, the strong adsorption film forming property of the corrosion inhibitor molecule is further improved, and the corrosion inhibitor has a good corrosion prevention effect under the environmental conditions that the temperature is higher than 150 ℃, the mineralization degree is higher than 20000mg/L, and CO2 and H2S are enriched.
In order to achieve the above object, the present invention provides the following technical solutions:
a high temperature resistant corrosion inhibitor has a structural formula shown as I:
wherein, the structural formula of R is shown as II:
the invention also provides a preparation method of the high-temperature-resistant corrosion inhibitor, which comprises the following steps:
s1, mixing trichlorotriazine with an organic solvent 1, refluxing, adding dimethylamine, carrying out reflux reaction for 10 hours, cooling, and concentrating under reduced pressure to obtain A;
s2, mixing chlorobutyric acid and dicyclohexylcarbodiimide, taking dichloromethane as a solvent, adding dopamine under the condition of stirring, reacting at 25 ℃ for more than 12 hours, precipitating with diethyl ether, and carrying out suction filtration to obtain B;
and S3, dissolving the B obtained in the step S2 in the organic solvent 2, dropwise adding the A obtained in the step S1 under a reflux condition, continuously refluxing for more than 24 hours after the dropwise adding is finished, cooling, concentrating under reduced pressure, precipitating with diethyl ether, and washing to obtain the high-temperature-resistant corrosion inhibitor.
Preferably, the organic solvent 1 in step S1 is ethanol or acetone.
Preferably, the molar ratio of the trichlorotriazine to the dimethylamine in the step S1 is 1:2-6; further preferably 1:4.
Preferably, the molar ratio of the chlorobutyric acid, dicyclohexylcarbodiimide and the dopamine in the step S2 is 1000:0.5-3:1000; further preferably 1000:1.5:1000.
Preferably, the organic solvent 2 in step S3 is acetone or chloroform.
Preferably, the washing is 3 times of washing the precipitate with absolute ethanol and diethyl ether, respectively.
The invention also provides application of the high-temperature-resistant corrosion inhibitor in shaft corrosion prevention.
Preferably, the temperature of the working condition environment of the application is 150-190 ℃, and the mineralization degree is 20000-250000mg/L.
Compared with the prior art, the invention has the beneficial effects that:
the invention improves the binding capacity of the corrosion inhibitor molecules and the metal surface by introducing triazine ring, benzene ring and hydroxyl into the corrosion inhibitor molecules, promotes the binding of the corrosion inhibitor molecules and the metal surface to be more compact, improves the binding site number of the corrosion inhibitor molecules and the metal surface, ensures the binding of the corrosion inhibitor molecules and the metal surface to be more extensive,the strong adsorption film forming property of the corrosion inhibitor molecules is improved, and the corrosion inhibition effect of the corrosion inhibitor molecules is improved. The mineralization degree is 20000-250000mg/L at 150-190 deg.C, and the corrosion inhibitor is rich in CO 2 And H 2 The corrosion inhibitor in the S environment reaches more than 85 percent.
Detailed Description
Embodiments of the present invention will be described below with reference to specific examples, and before the embodiments of the present invention are further described, it is to be understood that the scope of the present invention is not limited to the specific embodiments described below; it is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
The invention provides a high-temperature-resistant corrosion inhibitor, the structural formula of which is shown as I:
wherein, the structural formula of R is shown as II:
the triazine ring, benzene ring and hydroxyl are introduced into the corrosion inhibitor molecule, so that the binding capacity and the number of binding sites of the molecule and the metal surface are increased, the strong adsorption film forming property of the corrosion inhibitor molecule is further improved, and the mineralization degree is higher than 20000mg/L and the corrosion inhibitor is rich in CO at the temperature higher than 150 DEG C 2 And H 2 The S has better anti-corrosion effect under the environment condition.
Example 1 preparation of a high temperature Corrosion inhibitor
S1, adding 5mmol of trichlorotriazine into a three-port beaker, simultaneously adding 100ml of ethanol and 50ml of acetone as solvents, adding 20mmol of dimethylamine under the condition of reflux, carrying out reflux reaction for 10h, cooling, and concentrating under reduced pressure to obtain A;
s2, adding 20mol of chlorobutyric acid and 30mmol of dicyclohexylcarbodiimide into a three-port beaker, simultaneously adding 200ml of dichloromethane as a solvent, adding 20mol of dopamine under stirring, reacting at 25 ℃ for more than 12 hours, pouring the reaction product into diethyl ether with 3 times of volume to precipitate after the reaction is finished, and carrying out suction filtration to obtain B;
and S3, adding the B obtained in the step S2 into a three-port beaker, gradually dropwise adding the A obtained in the step S1 under the reflux condition by taking 100ml of acetone and 100ml of chloroform, continuously refluxing for more than 24 hours after the dropwise adding is finished, cooling, concentrating under reduced pressure, pouring into 100ml of diethyl ether for precipitation, and washing the precipitate for 3 times by using 50ml of absolute ethyl alcohol and 50ml of diethyl ether respectively to obtain a white solid, thereby obtaining the high-temperature-resistant corrosion inhibitor.
The nuclear magnetic resonance result of the obtained high-temperature corrosion inhibitor is as follows:
1H NMR(400MHz,CD3OD):6.72(3H,m,C6H3,H-9-12-13),3.66(2H,t,CONH-CH2,H-11),3.45(2H,t,N+-CH2,H-3),3.01(6H,s,N+-(CH3)2,H-2),2.76(2H,t,CH2-CONH,H-4),2.38(2H,t,C6H3-CH2,H-7)；
13C NMR(200MHz,CD3OD):176.5(s,C-5),162.1(s,C-1),148.6(s,C-10),148.1(s,C-11),135.5(s,C-8),126.1(s,C-13),119.8(s,C-9),116.2(s,C-12),65.6(t,C-3),51.1(q,C-2),43.2(t,C-6),38.2(t,C-7),29.9(t,C-4)。
EXAMPLE 2 preparation of high temperature Corrosion inhibitor
S1, adding 5mmol of trichlorotriazine into a three-port beaker, simultaneously adding 100ml of ethanol and 50ml of acetone as solvents, adding 10mmol of dimethylamine under the condition of reflux, carrying out reflux reaction for 10 hours, cooling, and concentrating under reduced pressure to obtain A;
s2, adding 20mol of chlorobutyric acid and 10mmol of dicyclohexylcarbodiimide into a three-port beaker, simultaneously adding 200ml of dichloromethane as a solvent, adding 20mol of dopamine under stirring, reacting at 25 ℃ for more than 12 hours, pouring the reaction product into diethyl ether with 3 times of volume to precipitate after the reaction is finished, and carrying out suction filtration to obtain B;
and S3, adding the B obtained in the step S2 into a three-port beaker, gradually dropwise adding the A obtained in the step S1 under the reflux condition by taking 100ml of acetone and 100ml of chloroform, continuously refluxing for more than 24 hours after the dropwise adding is finished, cooling, concentrating under reduced pressure, pouring into 100ml of diethyl ether for precipitation, and washing the precipitate for 3 times by using 50ml of absolute ethyl alcohol and 50ml of diethyl ether respectively to obtain a white solid, thereby obtaining the high-temperature-resistant corrosion inhibitor.
Example 3 preparation of a high temperature Corrosion inhibitor
S1, adding 5mmol of trichlorotriazine into a three-port beaker, simultaneously adding 100ml of ethanol and 50ml of acetone as solvents, adding 30mmol of dimethylamine under the condition of reflux, carrying out reflux reaction for 10h, cooling, and concentrating under reduced pressure to obtain A;
s2, adding 20mol of chlorobutyric acid and 60mmol of dicyclohexylcarbodiimide into a three-port beaker, simultaneously adding 200ml of dichloromethane as a solvent, adding 20mol of dopamine under stirring, reacting at 25 ℃ for more than 12 hours, pouring the reaction product into diethyl ether with 3 times of volume to precipitate after the reaction is finished, and carrying out suction filtration to obtain B;
and S3, adding the B obtained in the step S2 into a three-port beaker, gradually dropwise adding the A obtained in the step S1 under the reflux condition by taking 100ml of acetone and 100ml of chloroform, continuously refluxing for more than 24 hours after the dropwise adding is finished, cooling, concentrating under reduced pressure, pouring into 100ml of diethyl ether for precipitation, and washing the precipitate for 3 times by using 50ml of absolute ethyl alcohol and 50ml of diethyl ether respectively to obtain a white solid, thereby obtaining the high-temperature-resistant corrosion inhibitor.
The invention also provides application of the high-temperature-resistant corrosion inhibitor in shaft corrosion prevention.
Example 4 preparation of a high temperature Corrosion inhibitor
S1, adding 5mmol of trichlorotriazine into a three-port beaker, simultaneously adding 100ml of ethanol and 50ml of acetone as solvents, adding 25mmol of dimethylamine under the condition of reflux, carrying out reflux reaction for 10h, cooling, and concentrating under reduced pressure to obtain A;
s2, adding 20mol of chlorobutyric acid and 40mmol of dicyclohexylcarbodiimide into a three-port beaker, simultaneously adding 200ml of dichloromethane as a solvent, adding 20mol of dopamine under stirring, reacting at 25 ℃ for more than 12 hours, pouring the reaction product into diethyl ether with 3 times of volume to precipitate after the reaction is finished, and carrying out suction filtration to obtain B;
and S3, adding the B obtained in the step S2 into a three-port beaker, gradually dropwise adding the A obtained in the step S1 under the reflux condition by taking 100ml of acetone and 100ml of chloroform, continuously refluxing for more than 24 hours after the dropwise adding is finished, cooling, concentrating under reduced pressure, pouring into 100ml of diethyl ether for precipitation, and washing the precipitate for 3 times by using 50ml of absolute ethyl alcohol and 50ml of diethyl ether respectively to obtain a white solid, thereby obtaining the high-temperature-resistant corrosion inhibitor.
Comparative example 1
S1, adding 5mmol of trichlorotriazine into a three-port beaker, simultaneously adding 100ml of ethanol and 50ml of acetone as solvents, adding 5mmol of dimethylamine under the condition of reflux, carrying out reflux reaction for 10 hours, cooling, and concentrating under reduced pressure to obtain A;
s2, adding 20mol of chlorobutyric acid and 80mmol of dicyclohexylcarbodiimide into a three-port beaker, simultaneously adding 200ml of dichloromethane as a solvent, adding 15mol of dopamine under stirring, reacting at 25 ℃ for more than 12 hours, pouring the reaction product into diethyl ether with 3 times of volume to precipitate after the reaction is finished, and carrying out suction filtration to obtain B;
and S3, adding the B obtained in the step S2 into a three-port beaker, gradually dropwise adding the A obtained in the step S1 under the reflux condition by taking 100ml of acetone and 100ml of chloroform, continuously refluxing for more than 24 hours after the dropwise adding is finished, cooling, concentrating under reduced pressure, pouring into 100ml of diethyl ether for precipitation, and washing the precipitate for 3 times by using 50ml of absolute ethyl alcohol and 50ml of diethyl ether respectively to obtain a white solid, thereby obtaining the high-temperature-resistant corrosion inhibitor.
Comparative example 2
S1, adding 5mmol of trichlorotriazine into a three-port beaker, simultaneously adding 100ml of ethanol and 50ml of acetone as solvents, adding 32.5mmol of dimethylamine under the condition of reflux, carrying out reflux reaction for 10h, cooling, and concentrating under reduced pressure to obtain A;
s2, adding 20mol of chlorobutyric acid and 8mmol of dicyclohexylcarbodiimide into a three-port beaker, simultaneously adding 200ml of dichloromethane as a solvent, adding 15mol of dopamine under stirring, reacting at 25 ℃ for more than 12 hours, pouring the reaction product into diethyl ether with 3 times of volume to precipitate after the reaction is finished, and carrying out suction filtration to obtain B;
and S3, adding the B obtained in the step S2 into a three-port beaker, gradually dropwise adding the A obtained in the step S1 under the reflux condition by taking 100ml of acetone and 100ml of chloroform, continuously refluxing for more than 24 hours after the dropwise adding is finished, cooling, concentrating under reduced pressure, pouring into 100ml of diethyl ether for precipitation, and washing the precipitate for 3 times by using 50ml of absolute ethyl alcohol and 50ml of diethyl ether respectively to obtain a white solid, thereby obtaining the high-temperature-resistant corrosion inhibitor.
The invention also provides application of the high-temperature-resistant corrosion inhibitor in shaft corrosion prevention.
Specifically, the temperature of the working condition environment of the application is 150-190 ℃, and the mineralization degree is 20000-250000mg/L.
Experimental example 1
In the corrosive medium, the total mineralization is 28496.6mg/L, wherein K + +Na + 8380.2mg/L, ca 2+ 1990.5mg/L, mg 2+ 352.9mg/L, cl - 17087.4mg/L, SO 4 2- 70.8mg/L, HCO 3 - 574.5mg/L, I - The rotating speed of the P110 steel sheet is 20 revolutions per minute, the corrosion period is 7d, the total pressure is 15MPa, and the CO is the same as that of the steel sheet 2 、H 2 S、N 2 Under the conditions of partial pressures of 2, 1 and 12MPa respectively, when the using amount of the corrosion inhibitor is 300mg/L, the corrosion speed at different temperatures is evaluated, and the corrosion inhibition rate is calculated, and the results are shown in Table 1.
TABLE 1 Corrosion inhibition Properties of high temperature Corrosion inhibitors at different temperatures
As shown in the table, the high-temperature-resistant corrosion inhibitor prepared by the invention has a corrosion inhibition rate of 80.56-85.11% at 190 ℃, which indicates that the high-temperature-resistant performance of the corrosion inhibitor prepared by the invention is good. Meanwhile, according to comparative examples 1 and 2, the high temperature resistance of the corrosion inhibitor prepared when the mole ratio of trichlorotriazine to dimethylamine and the mole ratio of chlorobutyric acid, dicyclohexylcarbodiimide and dopamine are changed is poor, and the corrosion inhibition rate at 190 ℃ is only 49.36-50.21%, which indicates that changing the mole ratio of trichlorotriazine to dimethylamine and the mole ratio of chlorobutyric acid, dicyclohexylcarbodiimide and dopamine has an important influence on the high temperature resistance of the high temperature resistant corrosion inhibitor of the invention.
Experimental example two
In the corrosive medium, the total mineralization is 243063.1mg/L, wherein K + +Na + 70275.0mg/L, ca 2+ 10687.8mg/L, mg 2+ 1197.3mg/L, cl - 130606.3mg/L, SO4 2 -100.0 mg/L, HCO 3- 141.2mg/L, 20 rpm of P110 steel sheet, 7d corrosion period, 15MPa total pressure, CO 2 、H 2 S、N 2 Under the conditions of partial pressures of 2, 1 and 12MPa respectively, when the using amount of the corrosion inhibitor is 300mg/L, the corrosion speed at 180 ℃ is evaluated, and the corrosion inhibition rate is calculated, and the results are shown in Table 2.
TABLE 2
| Group of | Corrosion inhibition rate% |
| Blank control group | 0 |
| Example 1 | 87.86 |
| Example 2 | 82.35 |
| Example 3 | 80.93 |
| Example 4 | 85.72 |
| Comparative example 1 | 45.62 |
| Comparative example 2 | 48.10 |
As shown in the table, the corrosion inhibition rate of the high-temperature-resistant corrosion inhibitor prepared by the invention is 80.35-87.86% under the condition of extremely high mineralization, which indicates that the high-temperature-resistant corrosion inhibitor prepared by the invention is rich in CO at 180 ℃ under the condition of extremely high mineralization 2 And H 2 The S environment still shows good corrosion inhibition effect, wherein the high temperature resistant corrosion inhibitor prepared in the example 1 has the highest corrosion inhibition rate of 87.86%, which shows that the corrosion resistance is optimal.
The invention has been further described above in connection with specific embodiments, which are exemplary only and do not limit the scope of the invention in any way. It will be understood by those skilled in the art that various changes and substitutions of details and forms of the technical solution of the present invention may be made without departing from the spirit and scope of the present invention, but these changes and substitutions fall within the scope of the present invention.
Claims (5)
1. A high temperature resistant corrosion inhibitor has a structural formula shown as I:
wherein, the structural formula of R is shown as II:
2. the method for preparing the high temperature resistant corrosion inhibitor according to claim 1, comprising the following steps:
s1, mixing trichlorotriazine with an organic solvent 1, refluxing, adding dimethylamine, carrying out reflux reaction for 8-15h, cooling, and concentrating under reduced pressure to obtain A;
s2, mixing chlorobutyric acid and dicyclohexylcarbodiimide, taking dichloromethane as a solvent, adding dopamine under the condition of stirring, reacting at 25 ℃ for more than 12 hours, precipitating with diethyl ether, and carrying out suction filtration to obtain B;
s3, dissolving the B obtained in the step S2 in the organic solvent 2, dropwise adding the A obtained in the step S1 under a reflux condition, continuously refluxing for more than 24 hours after the dropwise adding is finished, cooling, concentrating under reduced pressure, precipitating with diethyl ether, and washing to obtain the high-temperature-resistant corrosion inhibitor;
the organic solvent 1 in the step S1 is ethanol and acetone; the molar ratio of the trichlorotriazine to the dimethylamine is 1:4;
the molar ratio of the chlorobutyric acid, dicyclohexylcarbodiimide and the dopamine in the step S2 is 1000:0.5-3:1000;
the organic solvent 2 in the step S3 is acetone and chloroform.
3. The method according to claim 2, wherein the washing is washing the precipitate 3 times with absolute ethanol and diethyl ether, respectively.
4. Use of the high temperature resistant corrosion inhibitor according to claim 1 or the high temperature resistant corrosion inhibitor prepared by the preparation method according to any one of claims 2 to 3 in wellbore corrosion protection.
5. The use according to claim 4, wherein the temperature of the working environment of the use is 150-190 ℃ and the mineralization degree is 20000-250000mg/L.
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