CN103059825B - Corrosion inhibitor for oil wells and preparation method - Google Patents
Corrosion inhibitor for oil wells and preparation method Download PDFInfo
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- CN103059825B CN103059825B CN201110317265.0A CN201110317265A CN103059825B CN 103059825 B CN103059825 B CN 103059825B CN 201110317265 A CN201110317265 A CN 201110317265A CN 103059825 B CN103059825 B CN 103059825B
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- inhibiter
- oil well
- alkyl phosphate
- corrosion inhibitor
- imidazolidine derivatives
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Abstract
The invention discloses a corrosion inhibitor for oil wells and a preparation method. The corrosion inhibitor includes the following components by weight: 20-40% of an imidazoline derivative, 25-35% of alkyl phosphate, 0.2-1% of thiourea, and the balance water. Specifically, the imidazoline derivative is prepared by subjecting imidazoline to water-soluble modification, and the alkyl phosphate has a molecular formula shown in the description, wherein n=4-20, and M=7-19. The method comprises: mixing and stirring the components uniformly according to the amounts so as to prepare the corrosion inhibitor for oil wells. The corrosion inhibitor provided in the invention can make corrosion inhibitor molecules arranged on a metal surface compactly, so that contact of the metal and a corrosive substance is greatly reduced, thus effectively inhibiting corrosion.
Description
Technical field
The present invention relates to field of oil drilling, say further, relate to a kind of oil well inhibiter and preparation method.
Background technology
Pit shaft and the relevant device of withdrawal well, based on waterflooding development, containing a large amount of mineral substance, bacterium etc. in the production water of oil field, are very easily corroded in current China oil field; CO is dissolved with in some oil wells production fluid
2, H
2the corrosive gasess such as S, corrosion condition is more serious.According to the literature, oil and petrochemical industry on average account for about 6% of the output value owing to corroding the loss caused.If take suitable safeguard procedures, 30% ~ 40% of corrosion loss can be retrieved.Current oil field suppresses the method for oil and water well corrosion to have: use the protection of extraordinary corrosion-resistant steel, coating for metal surfaces, electro-chemical protection, in corrosive medium, add inhibiter etc.; wherein add inhibiter and there is advantage not available for other guard method, easy to use, less investment, simple.Wherein the equal Zeng Zuowei inhibiter such as imidazolidine derivatives, PAPE, thiocarbamide, inorganic phosphate is used.Due to oil-field water complex structure, especially often containing CO
2, therefore corrosive medium complex, the limited efficiency of single inhibiter, is difficult to meet onsite application requirement, and the overwhelming majority is the composite use of multiple inhibiter.As CN00109688.5, CN02147875.9 etc. all describe imidazolidine derivatives as inhibiter, but must use together with alkynol, so just considerably increase cost.
Therefore, how to improve the effect of inhibiter, the cost reducing inhibiter is the current technical issues that need to address.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of oil well inhibiter and preparation method.Inhibitor molecular can be made at metallic surface dense arrangement, greatly reduce the contact of metal and corrosive deposit, thus the efficient generation suppressing corrosion.
An object of the present invention is to provide a kind of oil well inhibiter.
Comprise the following component with weight percent:
Imidazolidine derivatives 20-40%, alkyl phosphate 25-35%, thiocarbamide 0.2-1%, all the other are water,
Wherein, described imidazolidine derivatives is obtained through water-soluble modified by tetrahydroglyoxaline;
The molecular formula of described alkyl phosphate is:
Wherein n=4-20, preferred n=4-10, more preferably n=4; M=7-19, preferred m=8-10, more preferably m=8.
The preparation of described imidazolidine derivatives comprises:
(1) organic carboxyl acid and polyamines polyene are obtained by reacting imidazoline intermediate under the effect of organic solvent;
Organic carboxyl acid refers to C
11~ C
17saturated fatty acid, one or more in carboxylic acid, polyamines polyene is one or more in hydroxyethylethylene diamine, diethylenetriamine, triethylene tetramine;
The mol ratio of organic carboxyl acid and polyamines polyene is: 1: 1.05-1: 1.1, and temperature of reaction is 160-200 DEG C, the reaction times: 3-7 hour;
The molecular formula of described imidazoline intermediate is:
R
1for C
11~ C
17alkyl or phenyl, be preferably C
17h
33; R
2: amino, hydroxyl or thioureido, be preferably amino;
(2) imidazoline intermediate and modifying agent continue to be obtained by reacting imidazolidine derivatives;
Described modifying agent is the one in Glacial acetic acid, Mono Chloro Acetic Acid, thionamic acid;
The mol ratio of imidazoline intermediate and modifying agent is 1: 1-1: 1.05, and temperature of reaction is 100-140 DEG C, and the reaction times is 2-4 hour.
The concrete preparation of imidazolidine derivatives can adopt following steps:
(1) organic carboxyl acid and polyamines polyene are put into there-necked flask in molar ratio at 1: 1.05-1: 1.1, add appropriate organic solvent as azeotropic agent, heating, stirring, be warming up to 160-200 DEG C of reaction 3-7 hour, reaction end steams solvent, obtains imidazoline intermediate;
(2) by imidazoline intermediate and modifying agent with mol ratio for 1: 1-1: 1.05, put into there-necked flask, react 2-4 hour at 100-140 DEG C, namely obtain imidazolidine derivatives.
Described alkyl phosphate can adopt prior art to be obtained through Phosphation by polyethenoxy alkylphenols.
Specifically preferably can adopt following steps:
The mol ratio of polyethenoxy alkylphenols, water, Vanadium Pentoxide in FLAKES is 4: 3: 1, first polyethenoxy alkylphenols and water are added in there-necked flask, stir, under 40 DEG C of conditions, slowly add Vanadium Pentoxide in FLAKES while stirring, then 60-80 DEG C of reaction 5-8 hour, adds suitable quantity of water hydrolysis and namely obtains alkyl phosphate.
If other material can also be added in the special formula of the present invention of corrosive medium, as alkynol, phosphoric acid salt etc., can adjust as the case may be.
Two of object of the present invention is to provide a kind of preparation method of oil well inhibiter.
Comprise: described component is obtained described oil well inhibiter by described consumption mixing and stirring.
The present invention, by the rational proportion of each component, makes inhibitor molecular at metallic surface dense arrangement, greatly reduces the contact of metal and corrosive deposit, thus the efficient generation suppressing corrosion.Inhibiter provided by the invention can effectively suppress oil field production water to the corrosion of oil well, consumption 10-50mg/L, and corrosion inhibition rate is greater than 90%, year depth of corrosion be less than 0.076mm.
Embodiment
Below in conjunction with embodiment, further illustrate the present invention.
In embodiment raw materials used be commercially available.
The preparation of imidazolidine derivatives
(1) 0.15mol oleic acid, 0.16mol diethylenetriamine being put into there-necked flask, add 30mL dimethylbenzene as azeotropic agent, heating, stirring, be warming up to 180 DEG C of reactions 5 hours, judging whether reaction terminates by getting liquid survey infrared spectra; Reaction terminates rear rotatory evaporator and steams excess of solvent, obtains imidazoline intermediate (R
1c
17h
33, R
2amino).Imidazoline intermediate and Glacial acetic acid etc. mole are put into there-necked flask, reacts 2 hours at 120 DEG C, namely obtain imidazolidine derivatives 1#.
(2) 0.15mol oleic acid, 0.16mol hydroxyethylethylene diamine being put into there-necked flask, add 30mL dimethylbenzene as azeotropic agent, heating, stirring, be warming up to 180 DEG C of reactions 5 hours, judging whether reaction terminates by getting liquid survey infrared spectra; Reaction terminates rear rotatory evaporator and steams excess of solvent, obtains imidazoline intermediate (R
1c
17h
33, R
2hydroxyl).Imidazoline intermediate and thionamic acid etc. mole are put into there-necked flask, adds urea as catalyzer, react 2 hours at 120 DEG C, namely obtain imidazolidine derivatives 2#.
The preparation of alkyl phosphate
(1) under room temperature, be added in reactor by 0.1mol polyethenoxy alkylphenols (n=4, m=8), add water 0.075mol, stirs; Under 40 DEG C of conditions, add Vanadium Pentoxide in FLAKES 0.05mol while stirring, add in 1.5h.Then reaction system is heated to 70 DEG C of reaction 6h, adds appropriate water by product solid content demand, stir hydrolysis 30min at 60 DEG C and obtain alkyl phosphate 1#.
(2) under room temperature, be added in reactor by 0.1mol polyethenoxy alkylphenols (n=10, m=9), add water 0.075mol, stirs; Under 40 DEG C of conditions, add Vanadium Pentoxide in FLAKES 0.05mol while stirring, add in 1.5h.Then reaction system is heated to 70 DEG C of reaction 6h, adds appropriate water by product solid content demand, stir hydrolysis 30min at 60 DEG C and obtain alkyl phosphate 2#.
Evaluation method:
Evaluate corrosion inhibition by method of static coupon, evaluate the simulation salt solution that used medium is saturated carbonic acid gas, composition is in table 1.
Salt solution composition simulated by table 1
Experiment test piece process is with reference to oil and gas industry standard SY/T5273-2000 " oil field extracted water inhibiter method of evaluating performance ".In corrosive medium, add inhibiter, put into A3 steel disc, at 30 DEG C, place 72h, measure erosion rate and corrosion inhibition rate.
Embodiment 1:
Get above made imidazolidine derivatives 1#25g, alkyl phosphate 1#30g, thiocarbamide 0.5g, adds water to 100g, stirs, obtained inhibiter A.
The evaluation result of inhibiter A is in table 2:
Table 2 static steel experimental result
Embodiment 2:
Get above made imidazolidine derivatives 1#20g, alkyl phosphate 1#25g, thiocarbamide 1g, adds water to 100g, stirs, obtained inhibiter B.Evaluate corrosion inhibition by method of static coupon, evaluate the simulation salt solution that used medium is saturated carbonic acid gas, during consumption 50mg/L, erosion rate is 0.02548mm/a, and corrosion inhibition rate is 95.12%.
Embodiment 3:
Get above made imidazolidine derivatives 1#38g, alkyl phosphate 1#32g, thiocarbamide 0.2g, adds water to 100g, stirs, obtained inhibiter C.Evaluate corrosion inhibition by method of static coupon, evaluate the simulation salt solution that used medium is saturated carbonic acid gas, during consumption 50mg/L, erosion rate is 0.02105mm/a, and corrosion inhibition rate is 96.0%.
Embodiment 4:
Get above made imidazolidine derivatives 2#30g, alkyl phosphate 2#30g, thiocarbamide 0.3g, adds water to 100g, stirs, obtained inhibiter D.Evaluate corrosion inhibition by method of static coupon, evaluate the simulation salt solution that used medium is saturated carbonic acid gas, during consumption 50mg/L, erosion rate is 0.04217mm/a, and corrosion inhibition rate is 91.5%.
Embodiment 5:
Get above made imidazolidine derivatives 2#35g, alkyl phosphate 1#35g, thiocarbamide 0.2g, adds water to 100g, stirs, obtained inhibiter E.Evaluate corrosion inhibition by method of static coupon, evaluate the simulation salt solution that used medium is saturated carbonic acid gas, during consumption 50mg/L, erosion rate is 0.01217mm/a, and corrosion inhibition rate is 97.5%.
The erosion rate of inhibiter obtained in five embodiments is all less than 0.076mm/a; Corrosion inhibition rate is all greater than 90%, and therefore, inhibiter of the present invention, reduces the contact of metal and corrosive deposit greatly, thus the efficient generation suppressing corrosion, corrosion mitigating effect is good.
Claims (6)
1. an oil well inhibiter, is characterized in that: described inhibiter comprises the following component with weight percent:
Imidazolidine derivatives 20-40%, alkyl phosphate 25-35%, thiocarbamide 0.2-1%, all the other are water,
Wherein, described imidazolidine derivatives is obtained through water-soluble modified by tetrahydroglyoxaline;
The molecular formula of described alkyl phosphate is:
Wherein n=4-20, m=7-19;
The preparation of described imidazolidine derivatives comprises:
(1) organic carboxyl acid and polyamines polyene are obtained by reacting imidazoline intermediate under the effect of organic solvent;
Described organic carboxyl acid is C
11~ C
17saturated fatty acid in one or more, polyamines polyene is one or more in hydroxyethylethylene diamine, diethylenetriamine, triethylene tetramine;
(2) imidazoline intermediate and modifying agent continue to be obtained by reacting imidazolidine derivatives;
Described modifying agent is the one in Glacial acetic acid, Mono Chloro Acetic Acid, thionamic acid.
2. oil well inhibiter as claimed in claim 1, is characterized in that:
In step (1), the mol ratio of organic carboxyl acid and polyamines polyene is: 1:1.05-1:1.1, and temperature of reaction is 160-200 DEG C, and the reaction times is 3-7 hour;
In step (2), the mol ratio of imidazoline intermediate and modifying agent is 1:1-1:1.05, and temperature of reaction is 100-140 DEG C, and the reaction times is 2-4 hour.
3. oil well inhibiter as claimed in claim 1, is characterized in that:
In the molecular formula of described alkyl phosphate: n=4-10; M=8-10.
4. oil well inhibiter as claimed in claim 3, is characterized in that:
In the molecular formula of described alkyl phosphate: n=4; M=8.
5. oil well inhibiter as claimed in claim 1, is characterized in that:
Described alkyl phosphate is obtained through Phosphation by polyethenoxy alkylphenols.
6. a preparation method for the oil well inhibiter as described in one of Claims 1 to 5, comprising: described component is obtained described oil well inhibiter by described consumption mixing and stirring.
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104762626A (en) * | 2014-01-06 | 2015-07-08 | 天津中油科远石油工程有限责任公司 | Crude oil gathering and transportation corrosion inhibitor and preparation method thereof |
| CN103881684A (en) * | 2014-02-26 | 2014-06-25 | 中国石油化工股份有限公司 | Corrosion inhibitor used for CO2 foam flooding and preparation method thereof |
| CN104073810B (en) * | 2014-06-25 | 2016-04-13 | 西安石油大学 | For the oil-water media inhibiter of field produces oil gas water gathering system corrosion control |
| CN104829539B (en) * | 2015-04-13 | 2018-02-27 | 成都石大力盾科技有限公司 | Adipic acid bi-imidazoline derivative, the application of its preparation method and the derivative as corrosion inhibiter |
| CN105237698B (en) * | 2015-11-03 | 2017-11-17 | 天津亿利科能源科技发展股份有限公司 | Offshore oilfield water treatment system corrosion inhibiter and preparation method thereof |
| CN106086899B (en) * | 2016-08-16 | 2018-08-21 | 徐文忠 | For petrochemical industry H2S-HCl-CO2-HCN-H2The neutralization corrosion inhibitor of O etching systems |
| CN107502318A (en) * | 2017-08-08 | 2017-12-22 | 中国石油集团渤海钻探工程有限公司 | A kind of density brine completion fluid compound corrosion inhibitor and preparation method thereof |
| CN109440115B (en) * | 2018-10-31 | 2020-11-24 | 中国石油天然气集团公司 | Phosphoramidate water-soluble corrosion inhibitor and preparation method thereof |
| CN114854193B (en) * | 2022-03-28 | 2023-06-06 | 金发科技股份有限公司 | Polyamide composite material and preparation method and application thereof |
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| CN1966774A (en) * | 2006-09-04 | 2007-05-23 | 长庆石油勘探局 | Corrosion inhibitor resistant to H2S and CO2 |
| CN102020978A (en) * | 2010-12-22 | 2011-04-20 | 夹江县龙兴投资有限公司 | Gas well corrosion inhibitor and preparation method thereof |
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|---|---|---|---|---|
| CN1966774A (en) * | 2006-09-04 | 2007-05-23 | 长庆石油勘探局 | Corrosion inhibitor resistant to H2S and CO2 |
| CN102020978A (en) * | 2010-12-22 | 2011-04-20 | 夹江县龙兴投资有限公司 | Gas well corrosion inhibitor and preparation method thereof |
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| 辛基酚聚氧乙烯醚磷酸酯在钢表面的吸附与缓蚀作用;赵建国;《材料保护》;20080531;第41卷(第5期);第1.1和3节 * |
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