CN102586782A - Corrosion inhibitor and preparation and application thereof - Google Patents
Corrosion inhibitor and preparation and application thereof Download PDFInfo
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- CN102586782A CN102586782A CN2011100084287A CN201110008428A CN102586782A CN 102586782 A CN102586782 A CN 102586782A CN 2011100084287 A CN2011100084287 A CN 2011100084287A CN 201110008428 A CN201110008428 A CN 201110008428A CN 102586782 A CN102586782 A CN 102586782A
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Abstract
The invention discloses a corrosion inhibitor and preparation and application thereof. The corrosion inhibitor consists of the following components by total weight of the corrosion inhibitor: 1 to 15 weight percent of imidazoline ester, 1 to 10 weight percent of corrosion inhibition auxiliary and 5 to 50 weight percent of solvent. At a temperature of 30 to 130 DEG C, the corrosion inhibitor has good film forming property, has excellent dispersibility and solubility property and has the corrosion inhibition rate of over 86 percent under the condition of an additive amount of 20 to 50mg/L.
Description
Invention field
The present invention relates in the equipment of handling or transform hydrocarbon ils, add corrosion inhibitor, particularly a kind of anti-CO
2Corrosive inhibiter and preparation and application.
Background technology
In the performance history of oil and natural gas, CO
2Regular meeting is as associated gas while output, and the liquid phase corrosive medium that is accompanied by has gas well that white oil, oil-field water and composition thereof etc. are arranged usually.Along with the well water amount increases, deep layer contains CO
2The exploitation of hydrocarbon zone is increasing, notes CO
2The generally popularization of intensified technology for oil recovery, CO
2Corroding has become very distinct issues of of puzzlement oil and gas industry development at present, receives people's common concern.
Moist CO
2Can cause iron and steel general corrosion and serious local corrosion rapidly, make pipeline and hardware that early stage corrosion failure take place, cause enormous economic loss and serious societal consequence for the production and the transportation of oil gas.
Generally, anti-CO in the oil gas well
2The corrosive control techniques typically has following three kinds: select corrosion-resistant material, inside coating or lining, filling inhibiter.The practice at home and abroad experience shows, three kinds of technology, and inhibiter has that cost is low, simple to operate, instant effect, can protect integral device, be fit to characteristics such as long-term protection.The inhibiter resist technology as a kind of economy, effectively and the metallic corrosion control method of highly versatile, will be particularly suitable in oil gas well and gathering system, using.
At present about anti-CO
2Corrosive inhibiter patent is a lot, and its corrosion inhibition and range of application have their own characteristics each, and Chinese patent CN1818138A discloses a kind of inhibiter of being made up of oleic imidazolinone, thiocarbamide, water, Soxylat A 25-7, Virahol etc.; CN1410595A discloses a kind of inhibition carbon steel CO
2Corrosive water soluble rust inhibitor, its composition are mainly rosin Amine D, unit acid, thiocarbamide and verivate, solvent etc.; CN1277240A discloses a kind of oil field and has used novel anti CO
2Corrosion inhibitor, this inhibiter comprises: tetrahydroglyoxaline contains sulfur derivatives, alkyl phosphate, alkynol, nonionogenic tenside, solvent etc.; CN1966774A discloses a kind of inhibiter of being made up of Virahol, AEO, alkyl alcohol Soxylat A 25-7.
Above-mentioned inhibiter all can be applicable to the CO in oil-gas mining, the defeated process of collection
2Corrosion system, and good control CO is arranged
2The corrosive effect, but also have certain deficiency, the inhibiter use range that has is narrow, loses provide protection with the corrosion system variation of temperature; The inhibiter that has, film forming properties is unstable, and destructible is damaged; The inhibiter film forming properties that also has is good but water-soluble, poorly soluble; The inhibiter component that has is single, can't play composite synergy.
Summary of the invention
The present invention overcomes the deficiency of prior art, proposes a kind of inhibiter, the preparation method who the invention allows for a kind of inhibiter with its at oil gas well and gathering system CO
2Application in the corrosive environment.
A kind of inhibiter of the present invention, it is characterized by composed of the following components, in the inhibiter gross weight:
(A) fatty acid amide maleic acid ester 20～80 weight %
(B) imidazoline ester 1～25 weight %
(C) inhibition auxiliary agent 1～10 weight %
(D) solvent 5～50 weight %
The structural formula of described fatty acid amide maleic acid ester is:
Wherein: R
1Be C
10～C
20Alkyl or alkenyl.
Lipid acid in the described fatty acid amide is C
15～C
20The monocarboxylic acid of alkyl or alkenyl.
The structural formula of described imidazoline ester is:
Wherein: m=1～4; X=1～3, the positive integer of y=1～3.
Described inhibition auxiliary agent is at least a in thiocarbamide, propiolic alcohol, X 2073, the Sodium orthomolybdate, when the inhibition auxiliary agent is two or more, presses arbitrary proportion and mixes.
Described solvent is at least a in water, ethanol, methyl alcohol, the Virahol, when mixing more than both, presses arbitrary proportion and mixes.
A kind of preparation method of inhibition auxiliary agent, step is following:
1) preparation fatty acid amide maleic acid ester (A):
With C
15～C
20The lipid acid of alkyl or alkenyl and diethylolamine dropped in the reactor drum according to mol ratio in 1: 1～1: 4, stirred and were warming up to 140～220 ℃, fed N
2Gas refluxed 3～6 hours, reduced temperature of reaction to 70～120 ℃, C
15～C
20The lipid acid of alkyl or alkenyl and diethylolamine are according to 1: 1～1: 4 diethylolamine of mol ratio adding, and the catalyzer of 0.1～2 weight % is after the acid number of control product is constant; Reacted 3～6 hours; Be cooled to below 50 ℃,, add maleic anhydride according to mol ratio 1: 1～1: 2; 70～110 ℃ of reactions 3～8 hours, obtain the fatty acid amide maleic acid ester after the cooling;
Described catalyzer is NaOH, KOH, NaBH
4With in the sodium ethylate any one;
2) preparation of imidazoline ester:
With toluene or acetone is solvent, and imidazoles and the unsaturated dibasic acid esters that contains two keys are reacted, and its mol ratio is 1: 1～1: 2, and 50-90 ℃ of refluxed 12～24 hours, removing desolvates obtained imidazoline ester.
In the formula, m=1～4; X=1～3, y=1～3;
Described unsaturated ester is diethyl maleate, dibutyl maleate, 5-octene dicarboxylic acid dimethyl ester etc.;
3) with step 1) and step 2) 20～80 weight % (A) and 1～15 weight % (B) that obtain mix with the solvent of 1～10 weight % inhibition auxiliary agent and 5～50 weight %, inhibiter of the present invention.
A kind of application of inhibiter under 30～130 ℃ of conditions, is added inhibiter to CO with the addition of 20～50mg/L
2In the corrosive environment working fluid.Inhibition is to the corrosion of carbon steel equipment, and corrosion inhibition rate is more than 86%.
Inhibiter provided by the invention is compared with similar inhibiter; Have following characteristics: have a plurality of activated adsorption center; Contain a plurality of functional groups such as carboxyl, ester group, hydroxyl, carboxamido-group etc., and contain two keys such as C=N, C=C, C=O, therefore can pass through co-ordination bond, π key, two keys etc. and form chemisorption in the metallic surface; Even form the fine and close protective membrane of multiwalled, have economical and efficient property.This corrosion inhibitor product all has good corrosion inhibition in the range of temperature (30～130 ℃) of broad, need only can effectively control CO by 20～50mg/L
2Corrosive environment is to the corrosion of carbon steel equipment, and corrosion inhibition rate is more than 86%.
Make oil and gas pipes, gas well etc. at CO
2Obtain excellent protection in the corrosive medium, be applicable to 30～130 ℃ of the range of temperature of broad, this inhibiter film forming properties is better, has good dispersiveness and solubility property.The present invention provides characteristics such as the inhibiter consumption is few, the high and low poison ring of inhibition efficiency is protected, synthesis technique is simple in addition.
Embodiment
To combine the practical implementation instance that the present invention is described in further detail below, still, these embodiment are used for limiting by any way scope of the present invention.
Embodiment 1～7 is the preparation example of inhibiter;
Embodiment 8～10 is the static corrosion evaluation Example;
Embodiment 11 is the dynamic corrosion evaluation example of high temperature;
Embodiment 12 is the galvanic corrosion evaluation Example.
Embodiment 1～3 preparation component (A)
Embodiment 1
Oleic acid and diethylolamine are put in the reactor drum according to 1: 2 mol ratio, under constantly stirring, be warming up to 140～220 ℃, feed N
2Gas refluxed 3～6 hours, reduced temperature of reaction to 70～120 ℃, and added 1: 2 diethylolamine; And the NaOH of adding charging capacity 0.5%, with acid number control extent of reaction, obtain the fatty acid amide midbody; Continue reaction 3～6 hours, reaction was cooled to midbody below 50 ℃ after accomplishing, according to mol ratio 1: 1.1; Slowly add maleic anhydride in batches, add the back that finishes, obtain amine hydroxybenzene maleic acid ester (A) 1 after the cooling 70～110 ℃ of reactions 3～8 hours.
Embodiment 2
According to method like the preparation amine hydroxybenzene maleic acid ester category-A among the embodiment 1, add the KOH catalyzer of charging capacity 0.5%, replace oleic acid by palmitinic acid, make palmitic amide maleic acid ester (A) 2.
Embodiment 3
According to method like the preparation amine hydroxybenzene maleic acid ester category-A among the embodiment 1, the sodium ethylate catalyzer sodium ethylate that adds charging capacity 0.5% replaces oleic acid by linolic acid, makes linolic acid acid amides maleic acid ester (A) 3.
Embodiment 4～6 preparation components (B)
Embodiment 4
, as solvent the 0.1mol imidazoles is dissolved in the 50mL toluene with toluene, adds the diethyl maleate of 0.12mol again, 70 ℃ of refluxed 15 hours, underpressure distillation then, removing desolvates obtains imidazoline ester (B) 1.
Embodiment 5
According to the similar method of preparation imidazoline ester among the embodiment 4, replace diethyl maleate by dibutyl maleate, make imidazoline ester (B) 2.
Embodiment 6
According to the similar method of preparation imidazoline ester D among the embodiment 5, replace diethyl maleate by 5-octene dicarboxylic acid dimethyl ester, make imidazoline ester (B) 3.
Embodiment 7
According to making different fatty acid amide maleic acid esters, imidazoline ester, inhibition auxiliary agent and solvent among the embodiment 1～6 according to certainweight per-cent, compositely obtain different inhibiter, as shown in table 1.
The composition of the different inhibiter of table 1
Embodiment 8
Adopt constant temperature water bath, six mouthfuls of flasks (2000mL) to carry out CO
2The inhibiter static corrosion is estimated, and corrosive medium is CO
2(its preparation method is saturated solution: continuously logical N in the water
2Deoxygenation 1h feeds CO then
2Gas 1h reaches capacity until it), corrosion material 20G; Experimental period 48h; 60 ℃ of experimental temperatures.Investigate the corrosion inhibition (inhibiter derives from embodiment 7) of different inhibiter, experimental result is seen table 2.Can find out that from table 2 above-mentioned inhibiter is at CO
2All has corrosion inhibition preferably in the corrosive medium.
The static corrosion evaluation of the different inhibiter of table 2
Embodiment 9
Choose in the foregoing description 7 HSJ02 as inhibiter to be evaluated, change the inhibiter consumption, identical among evaluation method and the embodiment 8, investigation inhibiter add-on is to the influence of corrosion inhibition, and experimental result is seen table 3.
Table 3 density of corrosion inhibitor is to the influence of corrosion inhibition
From table 3, inhibiter uses lower concentration 20～50mg/L just can obtain reasonable corrosion mitigating effect, the anti-CO of this this inhibiter of explanation
2The corrosive excellent property.
Embodiment 10
Choose in the foregoing description 7 HSJ02 as inhibiter to be evaluated, change temperature, identical among evaluation method and the embodiment 8, the investigation temperature is to the influence of corrosion inhibition, and experimental result is seen table 4.
Can find out that from table 4 in 30～90 ℃ of scopes, corrosion inhibition rate embodies thermal adaptability and stability preferably all more than 90%.
Table 4 temperature is to the influence of corrosion inhibition
Embodiment 11
Adopt autoclave to carry out CO
2Corrosion evaluation test chooses that HSJ02 is as inhibiter to be evaluated in the foregoing description 7, and add-on is 50mg/L; Corrosive medium: CO
2Saturated solution; Temperature: 90 ℃, 100 ℃, 110 ℃, 120 ℃, 130 ℃; Test period: 96h; Rotating speed: 200r/min.
Testing sequence: in autoclave, add 1200mL zero(ppm) water, removing desolvates hangs test piece, feeds common N earlier
240min feeds high-purity N again
240min, and then logical CO
230min closes intake valve, air outlet valve then, heat temperature raising, be raised to preset temperature after, open intake valve, the beginning pressurising, be charged to predetermined pressure after, close inlet valve, pick up counting.
Test-results is seen table 5, from table 5, when temperature is 90～130 ℃, compares with low temperature, and corrosion inhibition rate slightly descends, but still more than 86%, corrosion mitigating effect is comparatively remarkable, and temperature variation is to its corrosion mitigating effect influence and not obvious.
Combine embodiment 10 again, in 30～130 ℃ of scopes, the inhibiter performance still has good suitability, and can keep stability preferably, and corrosion inhibition rate is greater than 86%.
Table 5 temperature is to the influence of corrosion inhibition
Embodiment 12
Adopt the Autolab electrochemical workstation to carry out the electrochemical measurement of inhibiter.Electrolyzer adopts three-electrode system, and Pt is a supporting electrode, and Ag/AgCl is a reference electrode, and (area is 0.78cm to cylindrical test piece (20G steel) for working electrode
2), experimental temperature is 60 ℃, corrosive medium is CO
2Saturated solution.It is electrolyzer that six mouthfuls of round-bottomed flasks are adopted in experiment, the water bath with thermostatic control controlled temperature.Working electrode is used epoxy encapsulation, and the workplace of the portion of only keeping on file is exposed in the solution, before the test, the bottom surface uses 240 respectively *, 400 *, 600 *, 800 * sand papering, use the acetone supersound washing.
During polarization curve was measured, sweep limit was-200～200mv, and sweep velocity is 0.0005V/s; Electrochemical impedance spectroscopy, actuation signal are the sine wave of 5mV, and its range of frequency is 1 * 10
5～1 * 10
-2Hz adopts the AutoLab analysis software to carry out data analysis.
The inhibiter HSJ02 that chooses among the embodiment 7 is the investigation object, and add-on is 50mg/L.
Impedance spectrum is a capacitive reactance arc basically, and the HSJ02 that adds 50mg/L concentration then demonstrates high frequency, the double-deck capacitive reactance arc of medium and low frequency.
Claims (10)
1. inhibiter is characterized in that: composed of the following components: in the inhibiter gross weight:
(A) fatty acid amide maleic acid ester 20～80 weight %
(B) imidazoline ester 1～25 weight %
(C) inhibition auxiliary agent 1～10 weight %
(D) solvent 5～50 weight %
In the inhibiter gross weight.
2. according to the described a kind of inhibiter of claim 1, it is characterized in that: the structural formula of component (A) fatty acid amide maleic acid ester is:
Wherein: R
1Be C
10～C
20Alkyl or alkenyl.
3. according to the described a kind of inhibiter of claim 1, it is characterized in that: the lipid acid in the described fatty acid amide is C
15～C
20The monocarboxylic acid of alkyl or alkenyl.
4. according to the described a kind of inhibiter of claim 1, it is characterized in that: the structural formula of described imidazoline ester is:
Wherein: m=1～4; X=1～3, the positive integer of y=1～3.
5. according to the described a kind of inhibiter of claim 1, it is characterized in that: described inhibition auxiliary agent is at least a in thiocarbamide, propiolic alcohol, X 2073, the Sodium orthomolybdate, when the inhibition auxiliary agent is two or more, presses arbitrary proportion and mixes.
6. according to the described a kind of inhibiter of claim 1, it is characterized in that: described solvent is at least a in water, ethanol, methyl alcohol, the Virahol, when mixing more than both, presses arbitrary proportion and mixes.
7. according to the preparation method of the described a kind of inhibiter of claim 1, it is characterized in that step is following:
1) preparation fatty acid amide maleic acid ester (A):
With C
15～C
20The lipid acid of alkyl or alkenyl and diethylolamine dropped in the reactor drum according to mol ratio in 1: 1～1: 4, stirred and were warming up to 140～220 ℃, fed N
2Gas refluxed 3～6 hours, reduced temperature of reaction to 70～120 ℃, C
15～C
20The lipid acid of alkyl or alkenyl and diethylolamine are according to 1: 1～1: 4 diethylolamine of mol ratio adding, and 0.1～2% catalyzer is after the acid number of control product is constant; Reacted 3～6 hours; Be cooled to below 50 ℃,, add maleic anhydride according to mol ratio 1: 1～1: 2; 70～110 ℃ of reactions 3～8 hours, obtain the fatty acid amide maleic acid ester after the cooling;
2) preparation of imidazoline ester:
With toluene or acetone is solvent, and imidazoles and the unsaturated dibasic acid esters that contains two keys are reacted, and imidazoles is 1: 1～1: 2 with the unsaturated dibasic acid esters mol ratio that contains two keys, and 50-90 ℃ of refluxed 12～24 hours, removing desolvates obtained imidazoline ester;
3) with step 1) and step 2) 20～80 weight % (A) and 1～15 weight % (B) that obtain mix with the solvent of 1～10 weight % inhibition auxiliary agent and 5～50 weight %, inhibiter of the present invention.
8. according to the preparation method of the described a kind of inhibiter of claim 7, it is characterized in that: described catalyzer is NaOH, KOH, NaBH
4With in the sodium ethylate any one.
9. according to the preparation method of the described a kind of inhibiter of claim 7, it is characterized in that: described unsaturated dibasic acid esters is diethyl maleate, dibutyl maleate, 5-octene dicarboxylic acid dimethyl ester.
10. according to the application of the described a kind of inhibiter of claim 7, it is characterized in that: under 30～130 ℃ of conditions, inhibiter added to the addition of 20～50mg/L contain CO
2In the corrosive environment working fluid.
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| 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 |
| CN103450866A (en) * | 2013-09-06 | 2013-12-18 | 中国海洋石油总公司 | High-temperature carbon dioxide corrosion inhibitor |
| CN109371401A (en) * | 2018-12-21 | 2019-02-22 | 陕西省石油化工研究设计院 | A kind of polyoxyethylene ether imidazoline sulfonate corrosion inhibiter and preparation method thereof |
| CN114806531A (en) * | 2021-01-29 | 2022-07-29 | 中国石油天然气股份有限公司 | High-flow-rate gathering and transportation corrosion inhibitor and preparation method and application thereof |
| CN115895627A (en) * | 2022-12-10 | 2023-04-04 | 河南中原石油助剂有限公司 | Sulfur-resistant corrosion inhibitor and preparation method thereof |
| WO2024092599A1 (en) * | 2022-11-03 | 2024-05-10 | Ecolab Usa Inc. | Corrosion-inhibiting additives and methods of making and use thereof |
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| CN103409129B (en) * | 2013-08-09 | 2016-04-27 | 上海富茵环保科技有限公司 | A kind of organic amine drilling well acidification corrosion inhibitor 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 |
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| CN103409122B (en) * | 2013-08-28 | 2015-09-23 | 中国石油集团川庆钻探工程有限公司 | Water-soluble corrosion inhibitor for resisting hydrogen sulfide |
| US9404189B2 (en) | 2013-09-06 | 2016-08-02 | China National Offshore Oil Corporation | High temperature carbon dioxide corrosion inhibitor |
| CN103450866B (en) * | 2013-09-06 | 2015-11-25 | 中国海洋石油总公司 | A kind of High-temperature carbon dioxide corrosion inhibitor |
| CN103450866A (en) * | 2013-09-06 | 2013-12-18 | 中国海洋石油总公司 | High-temperature carbon dioxide corrosion inhibitor |
| CN109371401A (en) * | 2018-12-21 | 2019-02-22 | 陕西省石油化工研究设计院 | A kind of polyoxyethylene ether imidazoline sulfonate corrosion inhibiter and preparation method thereof |
| CN109371401B (en) * | 2018-12-21 | 2021-03-23 | 陕西省石油化工研究设计院 | Polyoxyethylene ether imidazoline sulfonate corrosion inhibitor and preparation method thereof |
| CN114806531A (en) * | 2021-01-29 | 2022-07-29 | 中国石油天然气股份有限公司 | High-flow-rate gathering and transportation corrosion inhibitor and preparation method and application thereof |
| WO2024092599A1 (en) * | 2022-11-03 | 2024-05-10 | Ecolab Usa Inc. | Corrosion-inhibiting additives and methods of making and use thereof |
| CN115895627A (en) * | 2022-12-10 | 2023-04-04 | 河南中原石油助剂有限公司 | Sulfur-resistant corrosion inhibitor and preparation method thereof |
| CN115895627B (en) * | 2022-12-10 | 2023-10-31 | 河南中原石油助剂有限公司 | Sulfur-resistant corrosion inhibitor and preparation method thereof |
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Address after: 100728 Beijing, Chaoyangmen, North Street, No. 22, No. Applicant after: Sinopec Corp. Co-applicant after: Luoyang Petrochemical Engineering Corporation /SINOPEC Address before: 100728 Beijing, Chaoyangmen, North Street, No. 22, No. Applicant before: Sinopec Corp. Co-applicant before: Luoyang Petrochemical Engineering Co., China Petrochemical Group |
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