CN105154049B - A kind of corrosion inhibiter and preparation method thereof - Google Patents
A kind of corrosion inhibiter and preparation method thereof Download PDFInfo
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- CN105154049B CN105154049B CN201510471388.8A CN201510471388A CN105154049B CN 105154049 B CN105154049 B CN 105154049B CN 201510471388 A CN201510471388 A CN 201510471388A CN 105154049 B CN105154049 B CN 105154049B
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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 present invention relates to a kind of corrosion inhibiter and preparation method thereof.By weight percentage, the corrosion inhibiter includes：Mannich base 50~70%, phosphate 10~20%, isopropanol 10~20%, sodium molybdate 10~20%.The preparation method of the corrosion inhibiter is：N methylanilines are added in three-necked flask and are heated to 80 DEG C, pH value is adjusted to 2 with concentrated hydrochloric acid；Flask is heated to 95 DEG C, acetone is added into flask, is heated to 150 DEG C；Formaldehyde, benzaldehyde are added into flask, keeping temperature is 150 DEG C, stirs lower backflow 4 hours, obtains Mannich base；By weight percentage, Mannich base 50~70%, phosphate 10~20%, isopropanol 10~20%, sodium molybdate 10~20% are compounded, obtains corrosion inhibiter.The corrosion inhibiter is applicable to 180 DEG C of high temperature.When density of corrosion inhibitor is 100ppm, for system in Tahe Oilfield stratum aqueous corrosion of the N80 iron plates at 180 DEG C after 6 hours, the corrosion inhibition rate of corrosion inhibiter is 90.04%.
Description
Technical field
The present invention relates to oil-gas field development technical field, and in particular to a kind of water soluble rust inhibitor and preparation method thereof.
Background technology
The exploitation of extra-high temperature petroleum resources is always global problem, and cost of winning is high, and economic benefit is low, if oil gas provides
With corrosive gas such as hydrogen sulfide, carbon dioxide in source, Oil/gas Well tubing string, collect defeated circuit and will all face serious corrosion and ask
Topic.
At present solve etching problem thinking mainly have two, when change Oil/gas Well tubing string material make its corrosion-resistant or
Inside lining anti-corrosive tubing；Second, use corrosion inhibiter.In actual application, spot corrosion, pitting corrosion still occurs in corrosion-resistant tubing, by force
Degree can not just meet to produce needs in safe service life.Though corrosion inhibiter is commonly used, in high salinity media
The corrosion inhibiter still phoenix feathers and unicorn horns of high temperature resistance again, 150 DEG C domestic of corrosion inhibiter highest temperature resistance, has been difficult to meet Yuan Ba, tower at present
The inhibition demand of the high temperature Oil/gas Well such as river.Therefore, in order to ensure that the intensity of oil well pipe can normally meet production requirement, it is badly in need of
Invent a kind of Water-soluble high-temperature corrosion inhibitor for being applied to 180 DEG C of high temperature above.
The content of the invention
In order to solve the etching problem of Oil/gas Well tubing string in the exploitation of ultra-deep superhigh temperature petroleum resources, the present invention provides a kind of water
Dissolubility high-temperature corrosion inhibitor, by will Mannich base and phosphoric acid as made from methylphenylamine, acetone, formaldehyde, benzaldehyde, concentrated hydrochloric acid
Ester, isopropanol, sodium molybdate compounding, obtained corrosion inhibiter is applied to more than 180 DEG C of high temperature, so as to ultra-deep superhigh temperature Oil/gas Well
Metal tubing string is protected.
Specifically, the first technical scheme for using of the present invention is a kind of, corrosion inhibiter, by weight percentage, the high temperature
Corrosion inhibiter includes：Mannich base 50~70%, phosphate 10~20%, isopropanol 10~20%, sodium molybdate 10~20%, preferably
Ground, the corrosion inhibiter include：Mannich base 65%, phosphate 15%, isopropanol 10%, sodium molybdate 10%.
Foregoing corrosion inhibiter, the Mannich base is by the parts by weight of methylphenylamine 1, the parts by weight of acetone 1, the weight of formaldehyde 0.5
Part and the parts by weight of benzaldehyde 0.5 are made.
Foregoing corrosion inhibiter, the preparation method of the Mannich base comprise the following steps：
(1) parts by weight of methylphenylamine 1 are added in three-necked flask and are heated to 80 DEG C, pH value is adjusted to 2 with concentrated hydrochloric acid；
(2) flask is heated to 95 DEG C, the parts by weight of acetone 1 is added into flask, are heated to 150 DEG C；
(3) parts by weight of formaldehyde 0.5 and the parts by weight of benzaldehyde 0.5 are added into flask, keeping temperature is 150 DEG C, under stirring
Backflow 4 hours, obtains Mannich base.
Preferably, the preparation of the Mannich base is carried out under reflux.
Foregoing corrosion inhibiter, the preparation method of the Mannich base are further comprising the steps of：
(1) three-necked flask after backflow is cooled to room temperature, all substances therein is poured into beaker；
(2) beaker is heated to 180 DEG C while stirring, the constant temperature 3min at 180 DEG C；
(3) material in beaker is poured into three-necked flask, constant temperature flows back 1 hour at 180 DEG C, graceful after being purified
Buddhist nun wishes alkali.
The second technical scheme that the present invention uses is a kind of preparation method of corrosion inhibiter, this method comprises the following steps：
(1) parts by weight of methylphenylamine 1 are added in three-necked flask and are heated to 80 DEG C, pH value is adjusted to 2 with concentrated hydrochloric acid；
(2) solution is heated to 95 DEG C, the parts by weight of acetone 1 is added into flask, are heated to 150 DEG C；
(3) parts by weight of formaldehyde 0.5 and the parts by weight of benzaldehyde 0.5 are added into flask, keeping temperature is 150 DEG C, under stirring
Backflow 4 hours, obtains Mannich base；
(4) by weight percentage, by Mannich base 50~70%, phosphate 10~20%, isopropanol 10~20%, molybdenum
Sour sodium 10~20% is compounded, and obtains being applied to the corrosion inhibiter of 180 DEG C of high temperature；Preferably, by Mannich base 65%, phosphate
15%, isopropanol 10%, sodium molybdate 10% compounds, and obtains corrosion inhibiter.
The preparation method of foregoing corrosion inhibiter, the purification of Mannich base is also included after the step (3).
The preparation method of foregoing corrosion inhibiter, the purification of the Mannich base comprise the following steps：
(1) three-necked flask after backflow is cooled to room temperature, all substances therein is poured into beaker；
(2) beaker is heated while stirring, the constant temperature 3min at 180 DEG C；
(3) material in beaker is poured into three-necked flask, constant temperature flows back 1 hour at 180 DEG C, graceful after being purified
Buddhist nun wishes alkali.
The problem of Oil/gas Well tube corrosion is serious during the present invention exploits for extra-high temperature petroleum resources, it is proposed that Yi Zhonghuan
Agent and preparation method thereof is lost, by preparing Mannich base and it being purified, so that it is multiple with phosphate, isopropanol, sodium molybdate
Match somebody with somebody, obtained corrosion inhibiter can be in more than 180 DEG C applied at elevated temperature, and then control the mesh of the tube corrosion of high temperature oil gas well
's.
Embodiment
In order to be fully understood by the purpose of the present invention, feature and effect, by following embodiments, the present invention is made detailed
Describe in detail bright.For the process of the present invention in addition to the description below, remaining uses the conventional method or device of this area, chemical combination used
Raw material is the analysis pure compound of this area conventional commercial.
On the one hand, the invention provides a kind of corrosion inhibiter, by weight percentage, the corrosion inhibiter includes：Mannich base 50
~70%, phosphate 10~20%, isopropanol 10~20%, sodium molybdate 10~20%.
Preferably, corrosion inhibiter of the invention, by weight percentage, including：Mannich base 65%, phosphate 15% are different
Propyl alcohol 10%, sodium molybdate 10%.
Wherein, phosphate, isopropanol and sodium molybdate are mainly used in preventing and control high temperature spot corrosion, pitting corrosion.
Mannich base used in the present invention is by the parts by weight of methylphenylamine 1, the parts by weight of acetone 1, the parts by weight of formaldehyde 0.5 and benzene
The parts by weight of formaldehyde 0.5 are made.
Specifically, the preparation method of the Mannich base comprises the following steps：
(1) parts by weight of methylphenylamine 1 are added in three-necked flask, and electricity consumption heating mantle heats use concentrated hydrochloric acid to 80 DEG C
PH value is adjusted to 2；In addition to pH value is adjusted, concentrated hydrochloric acid also plays the effect of catalyst；
(2) flask is heated to 95 DEG C, the parts by weight of acetone 1 is added into flask, are heated to 150 DEG C；
(3) 0.5 parts by weight of formaldehyde and the parts by weight of benzaldehyde 0.5 are added into flask, keeping temperature is 150 DEG C, under stirring
Backflow 4 hours, obtains Mannich base；
Wherein, above-mentioned steps are carried out under condenser pipe backflow, and step (1) and (2) are flowed back using condenser pipe, on the one hand may be used
To keep pot temperature constant, component volatilization in flask on the other hand can be prevented.
Preferably, the preparation method of the Mannich base also includes following purification step：
(1) three-necked flask after backflow is cooled to room temperature, vapors away unreacted light component, then will be therein all
Material is poured into beaker；
(2) stirring magneton is put into beaker, is heated to 180 DEG C while stirring, makes beaker constant temperature 3min at 180 DEG C,
Flash distillation removes low temperature component；
(3) material in beaker is poured into three-necked flask, constant temperature flows back 1 hour at 180 DEG C, graceful after being purified
Buddhist nun wishes alkali.
On the other hand, the present invention also provides a kind of preparation method of corrosion inhibiter, and the preparation method is, with percentage by weight
Meter, the Mannich base 50~70% that the above method is prepared, phosphate 10~20%, isopropanol 10~20%, sodium molybdate
10~20% are compounded, and obtain corrosion inhibiter；Preferably, by Mannich base 65%, phosphate 15%, isopropanol 10%, molybdic acid
Sodium 10% compounds, and obtains corrosion inhibiter.
Above-mentioned preparation method is using the conventional preparation method in this area.
The corrosion inhibiter of the present invention is applicable to more than 180 DEG C of high temperature, and it is serious to solve existing Oil/gas Well tube corrosion
Problem.
It is right when dosage is 100ppm in 180 DEG C of high temperature Tahe oil field stratum water environments using the corrosion inhibiter of the present invention
The corrosion rate of N80 material iron plates is 0.0179mm/a, corrosion inhibition rate 90.04%.
Below, enumerate embodiment to further describe the present invention, but the present invention is not limited to following embodiments.
Embodiment
Illustrated first to raw materials used in embodiment：
| Raw material | Purity | Manufacturer |
| Methylphenylamine | Analyze pure | Nanjing Jin Long Chemical Co., Ltd.s |
| Acetone | Analyze pure | Tianjin Fu Yu Fine Chemical Co., Ltd |
| Formaldehyde | Analyze pure | Langfang Peng Cai Fine Chemical Co., Ltd |
| Benzaldehyde | Analyze pure | Jinzhong City development zone Zhong Zi Chemical Engineering Technologies Co., Ltd |
| Concentrated hydrochloric acid | Mass fraction 37.5%, analysis are pure | Its gloomy industrial chemicals of Yuanqu County's new city |
| Phosphate | Analyze pure | Hai'an petrochemical industry |
| Isopropanol | Analyze pure | Shanghai Dong Yi Chemical Co., Ltd.s |
| Sodium molybdate | Analyze pure | The crack chemical textile Co., Ltd in Wujiang |
Embodiment 1 prepares Mannich base
Methylphenylamine 10g, thermometer, the agitating device that device scope is 200 DEG C are added in 500ml three-necked flask
And reflux, electricity consumption heating mantle heats are to 80 DEG C, backflow, and the pH value of solution is adjusted to 2 with concentrated hydrochloric acid；Solution is continued to heat
To 95 DEG C, acetone 10g is added into flask, is heated to 150 DEG C；Formaldehyde 5g and benzaldehyde 5g, keeping temperature are added into flask
For 150 DEG C, lower backflow 4 hours is stirred, obtains Mannich base sample 1#.
Embodiment 2 prepares Mannich base
In 500ml three-necked flasks add methylphenylamine 10g, device scope be 200 DEG C thermometer, agitating device and
Reflux, electricity consumption heating mantle heats are to 80 DEG C, backflow, and the pH value of solution is adjusted to 2 with concentrated hydrochloric acid；Solution is continued to be heated to
95 DEG C, acetone 10g is added into flask, is heated to 150 DEG C；Formaldehyde 5g is added into flask and benzaldehyde 5g, keeping temperature are
150 DEG C, stir lower backflow 4 hours；Three-necked flask after backflow is cooled to room temperature, all substances therein are poured into 500ml
In beaker；Stirring magneton is put into beaker, 180 DEG C is heated to while stirring, makes beaker constant temperature 3min at 180 DEG C, will burn
Material in cup is poured into 500ml three-necked flasks, device reflux, and constant temperature flows back 1 hour at 180 DEG C, obtains Mannich
Alkali sample 2#.
Embodiment 3 prepares corrosion inhibiter
Mannich base sample 2#5.0g, phosphate 2.0g, isopropanol 1.0g, sodium molybdate 2.0g are compounded, delayed
Lose agent sample 1#.
Embodiment 4 prepares corrosion inhibiter
Mannich base sample 2#7.0g, phosphate 1.0g, isopropanol 1.0g, sodium molybdate 1.0g are compounded, delayed
Lose agent sample 2#.
Embodiment 5 prepares corrosion inhibiter
Mannich base sample 2#6.5g, phosphate 1.5g, isopropanol 1.0g, sodium molybdate 1.0g are compounded, delayed
Lose agent sample 3#.
The corrosion inhibiter corrosion inhibition of embodiment 6 is tested
Using People's Republic of China (PRC) chemical industry ministerial standard HG/T 2059~91 method to delaying made from embodiment 5
Lose agent sample 3# and carry out corrosion inhibition test, wherein agents useful for same and device is this area conventional commercial reagent and device.Prison
Survey under the corrosion inhibiter sample 3# protection that concentration is respectively 0ppm, 50ppm, 100ppm and 200ppm, the iron plate of N80 materials exists
Situation after the corrosion 6 hours of 180 DEG C of high temperature, while by market corrosion inhibiter sample A on sale and corrosion inhibiter sample B using same
The monitoring result that monitoring method obtains and corrosion inhibiter sample 3# monitoring result are contrasted, and monitoring result is as shown in table 1.Its
In, each component and its weight percent content in comparative sample A are：1- (two thiocarbamides)-ethyl -2- pentadecyl imidazolines
30%, octyl phosphate 25%, propilolic alcohol 10%, NONIN HS 240 15%, ethanol 20%；Comparative sample B is by coconut palm
What oleic acid, diethylenetriamine and dimethylbenzene were prepared.
Table 1
Note：Corrosion inhibition rate calculation formula：
η (%)=[(V1-V2)/V1]×100
In formula：η-corrosion inhibition rate, %
V1- the corrosion rate added before corrosion inhibiter, mm/a
V2- the corrosion rate added after corrosion inhibiter, mm/a
As shown in table 1, when no high-temperature corrosion inhibitor of the invention is protected, the corrosion rate of iron plate is 0.1798mm/a,
And when high-temperature corrosion inhibitor concentration is 100ppm, the corrosion rate of iron plate (disclosure satisfy that standard needs for 0.0179mm/a
0.076mm/a), corrosion inhibition rate 90.04%, and the corrosion inhibition rate of the comparative sample A and comparative sample B under same concentrations are only respectively
12.46% and 5.06%.Illustrate that the corrosion inhibiter of the present invention is protected for ultra-deep superhigh temperature Oil/gas Well metal tubing string, effectively control is high
The tube corrosion of warm Oil/gas Well.
The foregoing description of the disclosed embodiments, those skilled in the art are enable to realize or using the present invention.To this
A variety of modifications of a little embodiments will be apparent for a person skilled in the art, and generic principles defined herein can
Without departing from the spirit or scope of the present invention, to realize in other embodiments.Therefore, the present invention will not be limited
The embodiments shown herein is formed on, and is to fit to consistent with principles disclosed herein and features of novelty most wide
Scope.
Claims (7)
1. a kind of corrosion inhibiter, by weight percentage, the corrosion inhibiter include：Mannich base 50~70%, phosphate 10~20%,
Isopropanol 10~20%, sodium molybdate 10~20%；
Wherein, the Mannich base is by the parts by weight of methylphenylamine 1, the parts by weight of acetone 1, the parts by weight of formaldehyde 0.5 and benzaldehyde 0.5
Parts by weight are made；
Wherein, the preparation method of the Mannich base comprises the following steps：
(1) parts by weight of methylphenylamine 1 are added in three-necked flask and are heated to 80 DEG C, pH value is adjusted to 2 with concentrated hydrochloric acid；
(2) solution is heated to 95 DEG C, the parts by weight of acetone 1 is added into flask, are heated to 150 DEG C；
(3) parts by weight of formaldehyde 0.5 and the parts by weight of benzaldehyde 0.5 are added into flask, keeping temperature is 150 DEG C, stirs lower backflow 4
Hour, obtain Mannich base；
Wherein, the preparation method of the Mannich base is further comprising the steps of：
(1) three-necked flask after backflow is cooled to room temperature, all substances therein is poured into beaker；
(2) beaker is heated to 180 DEG C while stirring, the constant temperature 3min at 180 DEG C；
(3) material in beaker is poured into three-necked flask, constant temperature flows back 1 hour at 180 DEG C, the Mannich after being purified
Alkali.
2. corrosion inhibiter according to claim 1, it is characterised in that the described corrosion inhibiter includes：Mannich base 65%, phosphoric acid
Ester 15%, isopropanol 10%, sodium molybdate 10%.
3. corrosion inhibiter according to claim 1 or 2, it is characterised in that the preparation of the Mannich base is entered under reflux
OK.
A kind of 4. preparation method of corrosion inhibiter as described in any one of claims 1 to 3, it is characterised in that this method include with
Lower step：
(1) parts by weight of methylphenylamine 1 are added in three-necked flask and are heated to 80 DEG C, pH value is adjusted to 2 with concentrated hydrochloric acid；
(2) flask is heated to 95 DEG C, the parts by weight of acetone 1 is added into flask, are heated to 150 DEG C；
(3) parts by weight of formaldehyde 0.5 and the parts by weight of benzaldehyde 0.5 are added into flask, keeping temperature is 150 DEG C, stirs lower backflow 4
Hour, obtain Mannich base；
(4) by weight percentage, by Mannich base 50~70%, phosphate 10~20%, isopropanol 10~20%, sodium molybdate
10~20% are compounded, and obtain corrosion inhibiter.
5. the preparation method of corrosion inhibiter according to claim 4, it is characterised in that in step (4), with percentage by weight
Meter, Mannich base 65%, phosphate 15%, isopropanol 10%, sodium molybdate 10% are compounded, obtain corrosion inhibiter.
6. the preparation method of the corrosion inhibiter according to claim 4 or 5, it is characterised in that also include after the step (3) graceful
Buddhist nun wishes the purification of alkali.
7. the preparation method of corrosion inhibiter according to claim 6, it is characterised in that the purification of the Mannich base include with
Lower step：
(1) three-necked flask after backflow is cooled to room temperature, all substances therein is poured into beaker；
(2) beaker is heated to 180 DEG C while stirring, the constant temperature 3min at 180 DEG C；
(3) material in beaker is poured into three-necked flask, constant temperature flows back 1 hour at 180 DEG C, the Mannich after being purified
Alkali.
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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 |
| CN109810040B (en) | 2018-11-07 | 2020-02-18 | 西南石油大学 | Preparation method and application of Mannich base quaternary ammonium salt high-temperature-resistant acidizing corrosion inhibitor |
| 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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|---|---|---|---|---|
| CN1990912A (en) * | 2005-12-27 | 2007-07-04 | 中国石油化工股份有限公司 | Molybdenum phosphine system composite anti-erosion anti-sludging agent and preparation method thereof |
| CN103409129A (en) * | 2013-08-09 | 2013-11-27 | 上海富茵环保科技有限公司 | organic amine acidizing corrosion inhibitor used for well drilling and preparation method thereof |
| CN104805445A (en) * | 2015-03-24 | 2015-07-29 | 威海翔宇环保科技股份有限公司 | Environment-friendly copper corrosion inhibitor and preparation method thereof |
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2015
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| CN1990912A (en) * | 2005-12-27 | 2007-07-04 | 中国石油化工股份有限公司 | Molybdenum phosphine system composite anti-erosion anti-sludging agent and preparation method thereof |
| CN103409129A (en) * | 2013-08-09 | 2013-11-27 | 上海富茵环保科技有限公司 | organic amine acidizing corrosion inhibitor used for well drilling and preparation method thereof |
| CN104805445A (en) * | 2015-03-24 | 2015-07-29 | 威海翔宇环保科技股份有限公司 | Environment-friendly copper corrosion inhibitor and preparation method thereof |
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