CN105154049A - Corrosion inhibitor and preparation method thereof - Google Patents
Corrosion inhibitor and preparation method thereof Download PDFInfo
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- CN105154049A CN105154049A CN201510471388.8A CN201510471388A CN105154049A CN 105154049 A CN105154049 A CN 105154049A CN 201510471388 A CN201510471388 A CN 201510471388A CN 105154049 A CN105154049 A CN 105154049A
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- mannich base
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/54—Compositions for in situ inhibition of corrosion in boreholes or wells
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/32—Anticorrosion additives
Abstract
The invention relates to a corrosion inhibitor and a preparation method thereof. The corrosion inhibitor comprises, by weight: 50-70% of Mannich base, 10-20% of phosphate, 10-20% of isopropanol, and 10-20% of sodium molybdate. The preparation method of the corrosion inhibitor comprises: adding N-methylaniline into a three-neck flask, heating the flask to 80 DEG C, and adjusting the pH value to 2 with concentrated hydrochloric acid; heating the flask to 95 DEG C, adding acetone into the flask, and heating the flask to 150 DEG C; adding formaldehyde and benzaldehyde into the flask, maintaining the temperature at 150 DEG C, and performing reflux for 4h while performing stirring to obtain Mannich base; and compounding, by weight, 50-70% of Mannich base, 10-20% of phosphate, 10-20% of isopropanol, and 10-20% of sodium molybdate to prepare the corrosion inhibitor. The corrosion inhibitor can be used at a high temperature of 180 DEG C. When the concentration of the corrosion inhibitor is 100 ppm, an N80 iron sheet is corroded by stratum water of the Tahe Oilfield for 6h at 180 DEG C, and the corrosion inhibition rate is 90.04%.
Description
Technical field
The present invention relates to oil-gas field development technical field, be specifically related to a kind of water soluble rust inhibitor and preparation method thereof.
Background technology
The exploitation of extra-high temperature hydrocarbon resources is global problem always, and cost of winning is high, and economic benefit is low, if with the corrosive gases such as hydrogen sulfide, carbonic acid gas in hydrocarbon resources, Oil/gas Well tubing string, collection lines all will face serious etching problem.
The thinking of current solution etching problem mainly contains two, and one is change Oil/gas Well tubing string material to make its corrosion-resistant or inside lining anti-corrosive tubing; Two is use inhibiter.In actual application, corrosion-resistant tubing still there will be spot corrosion, pitting corrosion, and intensity just can not meet need of production in safe service life.Though inhibiter is generally applied, but in high salinity media the inhibiter of high temperature resistance still phoenix feathers and unicorn horns again, the highest temperature resistance of inhibiter domestic at present 150 DEG C, has been difficult to the inhibition demand of the high temperature Oil/gas Wells such as satisfied first dam, Tahe.Therefore, in order to ensure that the intensity of oil well pipe normally can meet Production requirement, be badly in need of a kind of Water-soluble high-temperature corrosion inhibitor being applicable to more than 180 DEG C high temperature of invention.
Summary of the invention
In order to solve the etching problem of Oil/gas Well tubing string in the exploitation of ultra-deep ultrahigh-temperature hydrocarbon resources; the invention provides a kind of Water-soluble high-temperature corrosion inhibitor; by will be composite by the obtained Mannich base of methylphenylamine, acetone, formaldehyde, phenyl aldehyde, concentrated hydrochloric acid and phosphoric acid ester, Virahol, Sodium orthomolybdate; the inhibiter obtained is applicable to the high temperature of more than 180 DEG C, thus protects ultra-deep ultrahigh-temperature Oil/gas Well metal tubing string.
Specifically, the first technical scheme that the present invention adopts is, a kind of inhibiter, by weight percentage, this high-temperature corrosion inhibitor comprises: Mannich base 50 ~ 70%, phosphoric acid ester 10 ~ 20%, Virahol 10 ~ 20%, Sodium orthomolybdate 10 ~ 20%, preferably, this inhibiter comprises: Mannich base 65%, phosphoric acid ester 15%, Virahol 10%, Sodium orthomolybdate 10%.
Aforesaid inhibiter, described Mannich base is made up of methylphenylamine 1 weight part, acetone 1 weight part, formaldehyde 0.5 weight part and phenyl aldehyde 0.5 weight part.
Aforesaid inhibiter, the preparation method of described Mannich base comprises the following steps:
(1) in there-necked flask, add methylphenylamine 1 weight part and be heated to 80 DEG C, by concentrated hydrochloric acid adjust ph to 2;
(2) flask is heated to 95 DEG C, in flask, adds acetone 1 weight part, be heated to 150 DEG C;
(3) in flask, add formaldehyde 0.5 weight part and phenyl aldehyde 0.5 weight part, keep temperature to be 150 DEG C, stir lower backflow 4 hours, obtain Mannich base.
Preferably, the preparation of described Mannich base is carried out all under reflux.
Aforesaid inhibiter, the preparation method of described Mannich base is further comprising the steps of:
(1) there-necked flask after backflow is cooled to room temperature, all substances are wherein poured in beaker;
(2) beaker is heated to 180 DEG C while stirring, constant temperature 3min at 180 DEG C;
(3) pour in there-necked flask by the material in beaker, at 180 DEG C, constant temperature refluxes 1 hour, obtains the Mannich base after purifying.
The second technical scheme that the present invention adopts is, a kind of preparation method of inhibiter, and the method comprises the following steps:
(1) in there-necked flask, add methylphenylamine 1 weight part and be heated to 80 DEG C, by concentrated hydrochloric acid adjust ph to 2;
(2) solution is heated to 95 DEG C, in flask, adds acetone 1 weight part, be heated to 150 DEG C;
(3) in flask, add formaldehyde 0.5 weight part and phenyl aldehyde 0.5 weight part, keep temperature to be 150 DEG C, stir lower backflow 4 hours, obtain Mannich base;
(4) by weight percentage, by Mannich base 50 ~ 70%, phosphoric acid ester 10 ~ 20%, Virahol 10 ~ 20%, Sodium orthomolybdate 10 ~ 20% carries out composite, obtains the inhibiter being applicable to 180 DEG C of high temperature; Preferably, by Mannich base 65%, phosphoric acid ester 15%, Virahol 10%, Sodium orthomolybdate 10% is composite, obtains inhibiter.
The preparation method of aforesaid inhibiter, also comprises the purification of Mannich base after described step (3).
The preparation method of aforesaid inhibiter, the purification of described Mannich base comprises the following steps:
(1) there-necked flask after backflow is cooled to room temperature, all substances are wherein poured in beaker;
(2) beaker is heated while stirring, constant temperature 3min at 180 DEG C;
(3) pour in there-necked flask by the material in beaker, at 180 DEG C, constant temperature refluxes 1 hour, obtains the Mannich base after purifying.
The present invention is directed to the problem that in the exploitation of extra-high temperature hydrocarbon resources, Oil/gas Well tube corrosion is serious, propose a kind of inhibiter and preparation method thereof, by preparing Mannich base and purifying to it, and then it is composite with phosphoric acid ester, Virahol, Sodium orthomolybdate, the inhibiter obtained can applied at elevated temperature more than 180 DEG C, and then reaches the object of the tube corrosion controlling high temperature oil gas well.
Embodiment
In order to fully understand object of the present invention, feature and effect, by following embodiment, the present invention is elaborated.Processing method of the present invention is except following content, and all the other all adopt ordinary method or the device of this area, and compound used therefor raw material is the analytical pure compound of this area conventional commercial.
On the one hand, the invention provides a kind of inhibiter, by weight percentage, this inhibiter comprises: Mannich base 50 ~ 70%, phosphoric acid ester 10 ~ 20%, Virahol 10 ~ 20%, Sodium orthomolybdate 10 ~ 20%.
Preferably, inhibiter of the present invention, by weight percentage, comprising: Mannich base 65%, phosphoric acid ester 15%, Virahol 10%, Sodium orthomolybdate 10%.
Wherein, phosphoric acid ester, Virahol and Sodium orthomolybdate are mainly used in the spot corrosion of prevention and corntrol high temperature, pitting corrosion.
The present invention's Mannich base used is made up of methylphenylamine 1 weight part, acetone 1 weight part, formaldehyde 0.5 weight part and phenyl aldehyde 0.5 weight part.
Particularly, the preparation method of described Mannich base comprises the following steps:
(1) in there-necked flask, add methylphenylamine 1 weight part, and electricity consumption heating mantle heats to 80 DEG C, by concentrated hydrochloric acid adjust ph to 2; Except adjust ph, concentrated hydrochloric acid also serves the effect of catalyzer;
(2) flask is heated to 95 DEG C, in flask, adds acetone 1 weight part, be heated to 150 DEG C;
(3) in flask, add 0.5 parts by weight of formaldehyde and phenyl aldehyde 0.5 weight part, keep temperature to be 150 DEG C, stir lower backflow 4 hours, obtain Mannich base;
Wherein, above-mentioned steps is all carried out under prolong backflow, and step (1) and (2) adopt prolong backflow, pot temperature can be kept constant on the one hand, can prevent component volatilization in flask on the other hand.
Preferably, the preparation method of described Mannich base also comprises following purification step:
(1) there-necked flask after backflow is cooled to room temperature, vapors away unreacted light constituent, then all substances are wherein poured in beaker;
(2) stirring magneton is put into beaker, be heated to 180 DEG C while stirring, make beaker constant temperature 3min at 180 DEG C, low temperature component is removed in flash distillation;
(3) pour in there-necked flask by the material in beaker, at 180 DEG C, constant temperature refluxes 1 hour, obtains the Mannich base after purifying.
On the other hand, the present invention also provides a kind of preparation method of inhibiter, and this preparation method is, by weight percentage, the Mannich base 50 ~ 70% that aforesaid method is prepared, phosphoric acid ester 10 ~ 20%, Virahol 10 ~ 20%, Sodium orthomolybdate 10 ~ 20% carries out composite, obtains inhibiter; Preferably, by Mannich base 65%, phosphoric acid ester 15%, Virahol 10%, Sodium orthomolybdate 10% is composite, obtains inhibiter.
Above-mentioned preparation method adopts the preparation method of this area routine.
Inhibiter of the present invention is applicable to the high temperature of more than 180 DEG C, solves the difficult problem that existing Oil/gas Well tube corrosion is serious.
Adopt inhibiter of the present invention, in 180 DEG C of high temperature system in Tahe Oilfield local water environment, when dosage is 100ppm, be 0.0179mm/a to the erosion rate of N80 material iron plate, corrosion inhibition rate is 90.04%.
Below, enumerate embodiment and the present invention is further described, but the present invention is not limited to following embodiment.
Embodiment
First be described raw materials used in embodiment:
| Raw material | Purity | Manufacturer |
| Methylphenylamine | Analytical pure | Nanjing Jin Long Chemical Co., Ltd. |
| Acetone | Analytical pure | Tianjin Fu Yu Fine Chemical Co., Ltd |
| Formaldehyde | Analytical pure | Langfang Peng Cai Fine Chemical Co., Ltd |
| Phenyl aldehyde | Analytical pure | Development area, Jinzhong City Zhong Zi Chemical Engineering Technology company limited |
| Concentrated hydrochloric acid | Massfraction 37.5%, analytical pure | Its gloomy industrial chemicals of Yuanqu County's new city |
| Phosphoric acid ester | Analytical pure | Hai'an petrochemical industry |
| Virahol | Analytical pure | Shanghai Dong Yi Chemical Co., Ltd. |
| Sodium orthomolybdate | Analytical pure | The crack chemical textile company limited in Wujiang |
Embodiment 1 prepares Mannich base
In the there-necked flask of 500ml, add methylphenylamine 10g, device scope is thermometer, whipping appts and the reflux of 200 DEG C, electricity consumption heating mantle heats to 80 DEG C, backflow, by the pH value of concentrated hydrochloric acid regulator solution to 2; Solution is continued be heated to 95 DEG C, in flask, add acetone 10g, be heated to 150 DEG C; In flask, add formaldehyde 5g and phenyl aldehyde 5g, keep temperature to be 150 DEG C, stir lower backflow 4 hours, obtain Mannich base sample 1#.
Embodiment 2 prepares Mannich base
In 500ml there-necked flask, add methylphenylamine 10g, device scope is thermometer, whipping appts and the reflux of 200 DEG C, electricity consumption heating mantle heats to 80 DEG C, backflow, by the pH value of concentrated hydrochloric acid regulator solution to 2; Solution is continued be heated to 95 DEG C, in flask, add acetone 10g, be heated to 150 DEG C; In flask, add formaldehyde 5g and phenyl aldehyde 5g, keep temperature to be 150 DEG C, stir lower backflow 4 hours; There-necked flask after backflow is cooled to room temperature, all substances is wherein poured in 500ml beaker; Stirring magneton is put into beaker, is heated to 180 DEG C while stirring, make beaker constant temperature 3min at 180 DEG C, poured into by the material in beaker in 500ml there-necked flask, device reflux, at 180 DEG C, constant temperature refluxes 1 hour, obtains Mannich base sample 2#.
Embodiment 3 prepares inhibiter
By Mannich base sample 2#5.0g, phosphoric acid ester 2.0g, Virahol 1.0g, Sodium orthomolybdate 2.0g carries out composite, obtains inhibiter sample 1#.
Embodiment 4 prepares inhibiter
By Mannich base sample 2#7.0g, phosphoric acid ester 1.0g, Virahol 1.0g, Sodium orthomolybdate 1.0g carries out composite, obtains inhibiter sample 2#.
Embodiment 5 prepares inhibiter
By Mannich base sample 2#6.5g, phosphoric acid ester 1.5g, Virahol 1.0g, Sodium orthomolybdate 1.0g carries out composite, obtains inhibiter sample 3#.
Embodiment 6 inhibiter corrosion inhibition is tested
The inhibiter sample 3# adopting the method for People's Republic of China's chemical industry ministerial standard HG/T2059 ~ 91 obtained to embodiment 5 carries out corrosion inhibition test, and wherein agents useful for same and device are this area conventional commercial reagent and device.Under monitoring the protection of inhibiter sample 3# being respectively 0ppm, 50ppm, 100ppm and 200ppm in concentration; the iron plate of N80 material is in the situation of corrosion after 6 hours of 180 DEG C of high temperature; the monitoring result simultaneously adopting same monitoring method to obtain inhibiter sample A on sale for market and inhibiter sample B and the monitoring result of inhibiter sample 3# contrast, and monitoring result is as shown in table 1.Wherein, each component in comparative sample A and weight percent content thereof are: 1-(two thiocarbamides)-ethyl-2-pentadecyl tetrahydroglyoxaline 30%, octyl phosphate 25%, propiolic alcohol 10%, polyoxyethylene octyl phenyl ether 15%, ethanol 20%; Comparative sample B is prepared by coconut oil, diethylenetriamine and dimethylbenzene.
Table 1
Note: corrosion inhibition rate calculation formula:
η(％)＝[(V
1-V
2)/V
1]×100
In formula: η-corrosion inhibition rate, %
V
1-add the erosion rate before inhibiter, mm/a
V
2-add the erosion rate after inhibiter, mm/a
As shown in table 1; when not having high-temperature corrosion inhibitor of the present invention to protect; the erosion rate of iron plate is 0.1798mm/a; and when high-temperature corrosion inhibitor concentration is 100ppm; the erosion rate of iron plate is 0.0179mm/a (can meet standard needs 0.076mm/a); corrosion inhibition rate is 90.04%, and the corrosion inhibition rate of comparative sample A under same concentrations and comparative sample B is only 12.46% and 5.06% respectively.Illustrate that inhibiter of the present invention is for the protection of ultra-deep ultrahigh-temperature Oil/gas Well metal tubing string, effectively controls the tube corrosion of high temperature oil gas well.
To the above-mentioned explanation of the disclosed embodiments, those skilled in the art are realized or uses the present invention.To be apparent for a person skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (9)
1. an inhibiter, by weight percentage, this inhibiter comprises: Mannich base 50 ~ 70%, phosphoric acid ester 10 ~ 20%, Virahol 10 ~ 20%, Sodium orthomolybdate 10 ~ 20%, preferably, this inhibiter comprises: Mannich base 65%, phosphoric acid ester 15%, Virahol 10%, Sodium orthomolybdate 10%.
2. inhibiter according to claim 1, is characterized in that, described Mannich base is made up of methylphenylamine 1 weight part, acetone 1 weight part, formaldehyde 0.5 weight part and phenyl aldehyde 0.5 weight part.
3. inhibiter according to claim 1 and 2, is characterized in that, the preparation method of described Mannich base comprises the following steps:
(1) in there-necked flask, add methylphenylamine 1 weight part and be heated to 80 DEG C, by concentrated hydrochloric acid adjust ph to 2;
(2) solution is heated to 95 DEG C, in flask, adds acetone 1 weight part, be heated to 150 DEG C;
(3) in flask, add formaldehyde 0.5 weight part and phenyl aldehyde 0.5 weight part, keep temperature to be 150 DEG C, stir lower backflow 4 hours, obtain Mannich base.
4. inhibiter according to claim 3, is characterized in that, the preparation method of described Mannich base is further comprising the steps of:
(1) there-necked flask after backflow is cooled to room temperature, all substances are wherein poured in beaker;
(2) beaker is heated to 180 DEG C while stirring, constant temperature 3min at 180 DEG C;
(3) pour in there-necked flask by the material in beaker, at 180 DEG C, constant temperature refluxes 1 hour, obtains the Mannich base after purifying.
5. inhibiter according to claim 3, is characterized in that, the preparation of described Mannich base is carried out all under reflux.
6. a preparation method for the inhibiter as described in any one of Claims 1 to 5, is characterized in that, the method comprises the following steps:
(1) in there-necked flask, add methylphenylamine 1 weight part and be heated to 80 DEG C, by concentrated hydrochloric acid adjust ph to 2;
(2) flask is heated to 95 DEG C, in flask, adds acetone 1 weight part, be heated to 150 DEG C;
(3) in flask, add formaldehyde 0.5 weight part and phenyl aldehyde 0.5 weight part, keep temperature to be 150 DEG C, stir lower backflow 4 hours, obtain Mannich base;
(4) by weight percentage, by Mannich base 50 ~ 70%, phosphoric acid ester 10 ~ 20%, Virahol 10 ~ 20%, Sodium orthomolybdate 10 ~ 20% carries out composite, obtains inhibiter.
7. the preparation method of inhibiter according to claim 6, is characterized in that, in step (4), by weight percentage, by Mannich base 65%, phosphoric acid ester 15%, Virahol 10%, Sodium orthomolybdate 10% is composite, obtains inhibiter.
8. the preparation method of the inhibiter according to claim 6 or 7, is characterized in that, also comprises the purification of Mannich base after described step (3).
9. the preparation method of inhibiter according to claim 8, is characterized in that, the purification of described Mannich base comprises the following steps:
(1) there-necked flask after backflow is cooled to room temperature, all substances are wherein poured in beaker;
(2) beaker is heated to 180 DEG C while stirring, constant temperature 3min at 180 DEG C;
(3) pour in there-necked flask by the material in beaker, at 180 DEG C, constant temperature refluxes 1 hour, obtains the Mannich base after purifying.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107987822A (en) * | 2017-12-06 | 2018-05-04 | 唐山市金沙工贸有限公司 | High-temperature acidification corrosion inhibitor and preparation method thereof and application |
| WO2020093444A1 (en) * | 2018-11-07 | 2020-05-14 | 西南石油大学 | Method for preparing mannich base quaternary ammonium salt-based high temperature resistant acidizing corrosion inhibitor and use of same |
| CN114214052A (en) * | 2021-12-13 | 2022-03-22 | 中海石油(中国)有限公司 | Compound corrosion inhibitor for high-density completion fluid in micro-sulfur-containing environment and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107987822A (en) * | 2017-12-06 | 2018-05-04 | 唐山市金沙工贸有限公司 | High-temperature acidification corrosion inhibitor and preparation method thereof and application |
| WO2020093444A1 (en) * | 2018-11-07 | 2020-05-14 | 西南石油大学 | Method for preparing mannich base quaternary ammonium salt-based high temperature resistant acidizing corrosion inhibitor and use of same |
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| CN114214052A (en) * | 2021-12-13 | 2022-03-22 | 中海石油(中国)有限公司 | Compound corrosion inhibitor for high-density completion fluid in micro-sulfur-containing environment and preparation method and application thereof |
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