CN102586782B - Corrosion inhibitor and preparation and application thereof - Google Patents

Corrosion inhibitor and preparation and application thereof Download PDF

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CN102586782B
CN102586782B CN201110008428.7A CN201110008428A CN102586782B CN 102586782 B CN102586782 B CN 102586782B CN 201110008428 A CN201110008428 A CN 201110008428A CN 102586782 B CN102586782 B CN 102586782B
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inhibiter
ester
preparation
corrosion
acid
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CN102586782A (en
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唐应彪
李朝法
段永锋
李春贤
孙新乐
刘强
石运峰
张庆源
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China Petroleum and Chemical Corp
Sinopec Luoyang Guangzhou Engineering Co Ltd
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Sinopec Luoyang Petrochemical Engineering Corp
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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

A kind of inhibiter and preparation thereof and application
Invention field
The present invention relates to add corrosion inhibitor in the equipment of processing or coverting hydrocarbon oils, particularly a kind of anti-CO 2inhibiter and preparation and the application of corrosion.
Background technology
In the performance history of oil and natural gas, CO 2often can be as associated gas while output, the liquid phase corrosive medium be accompanied by has gas well that condensate oil, oil-field water and composition thereof etc. are arranged usually.Along with water content of oil well increases, deep layer contains CO 2the exploitation of hydrocarbon zone is increasing, notes CO 2the generally popularization of intensified oil reduction technique, CO 2corrode and become very distinct issues of of puzzlement oil and gas industry development at present, be subject to 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 occur, cause huge financial loss and serious societal consequence to production and the transportation of oil gas.
Generally, anti-CO in Oil/gas Well 2the control techniques of corrosion 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 applicable to the 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 for applying in Oil/gas Well and gathering system.
At present about anti-CO 2the inhibiter patent of corrosion 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 be comprised of oleic imidazolinone, thiocarbamide, water, Soxylat A 25-7, Virahol etc.; CN1410595A discloses a kind of inhibition carbon steel CO 2the water soluble rust inhibitor of corrosion, its composition is mainly rosin Amine D, unit acid, thiocarbamide and derivative, solvent etc.; CN1277240A discloses novel anti-CO for a kind of oil field 2corrosion inhibitor, this inhibiter comprises: tetrahydroglyoxaline is containing sulfur derivatives, alkyl phosphate, alkynol, nonionogenic tenside, solvent etc.; CN1966774A discloses a kind of inhibiter be comprised of Virahol, fatty alcohol-polyoxyethylene ether, alkyl alcohol Soxylat A 25-7.
Above-mentioned inhibiter all can be applicable to oil-gas mining, collects the CO in defeated process 2corrosion system, and good control CO is arranged 2, but also there is certain deficiency in the effect of corrosion, and some inhibiter use range are narrow, with the variation of corrosion system temperature, loses provide protection; Some inhibiter, film forming properties is unstable, and destructible is damaged; The inhibiter film forming properties also had is good but water-soluble, poorly soluble; Some inhibiter components are single, can't play composite synergy.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, proposes a kind of inhibiter, the invention allows for a kind of preparation method of inhibiter and it is at Oil/gas Well and gathering system CO 2application in 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 % by weight
(B) imidazoline ester 1～25 % by weight
(C) inhibition auxiliary agent 1～10 % by weight
(D) solvent 5～50 % by weight
The structural formula of described fatty acid amide maleic acid ester is:
Wherein: R 1for C 10～C 20alkyl or alkenyl.
Lipid acid in described fatty acid amide is C 15～C 20the monocarboxylic acid of alkyl or alkenyl.
The structural formula of described imidazoline ester is:
Figure BSA00000419185800031
Wherein: m=1～4; X=1～3, the positive integer of y=1～3.
Described inhibition auxiliary agent is at least one in thiocarbamide, propiolic alcohol, Sodium dodecylbenzene sulfonate, Sodium orthomolybdate, when the inhibition auxiliary agent is two or more, mixes in any proportion.
Described solvent is at least one in water, ethanol, methyl alcohol, Virahol, during both above mixing, mixes in any proportion.
A kind of preparation method of inhibition auxiliary agent, step is as follows:
1) prepare fatty acid amide maleic acid ester (A):
By C 15～C 20the lipid acid of alkyl or alkenyl and diethanolamine drop in reactor according to mol ratio in 1: 1～1: 4, stir and are warming up to 140～220 ℃, pass into N 2gas, reflux 3～6 hours, reduces temperature of reaction to 70～120 ℃, C 15～C 20the lipid acid of alkyl or alkenyl and diethanolamine add the diethanolamine of 1: 1～1: 4 according to mol ratio, 0.1 the catalyzer of～2 % by weight, after the acid number of control product is constant, react 3～6 hours, be cooled to below 50 ℃, according to mol ratio 1: 1～1: 2, add maleic anhydride, 70～110 ℃ of reactions 3～8 hours, obtain the fatty acid amide maleic acid ester after cooling;
Described catalyzer is NaOH, KOH, NaBH 4with any one in sodium ethylate;
2) preparation of imidazoline ester:
Take toluene or acetone as solvent, imidazoles is reacted with the unsaturated dibasic acid esters that contains two keys, its mol ratio is 1: 1～1: 2, under 50-90 ℃, refluxes 12～24 hours, except desolventizing obtains imidazoline ester.
Figure BSA00000419185800032
In 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) by step 1) and step 2) 20～80 % by weight (A) and 1～15 % by weight (B) that obtain mixed with the solvent of 1～10 % by weight inhibition auxiliary agent and 5～50 % by weight, obtains inhibiter of the present invention.
A kind of application of inhibiter, under 30～130 ℃ of conditions, add inhibiter to CO with the addition of 20～50mg/L 2in the corrosive environment working fluid.The corrosion of inhibition to carbon steel equipment, corrosion inhibition rate is more than 86%.
Inhibiter provided by the invention is compared with similar inhibiter; there is following characteristics: there is a plurality of activated adsorption center; contain a plurality of functional groups as carboxyl, ester group, hydroxyl, amide group etc.; and containing two keys such as C=N, C=C, C=O; therefore can pass through coordinate bond, π key, two keys etc. and form chemisorption in metallic surface; even form the fine and close protective membrane of multilayer, there is economical and efficient.This corrosion inhibitor product all has good corrosion inhibition in wider range of temperature (30～130 ℃), need only can effectively control CO by 20～50mg/L 2the corrosion of corrosive environment to carbon steel equipment, corrosion inhibition rate is more than 86%.
Make oil and gas pipes, gas well etc. at CO 2obtain good protection in corrosive medium, be applicable to 30～130 ℃ of wider range of temperature, this inhibiter film forming properties is better, has good dispersiveness and solubility property.The invention provides in addition the characteristics such as the inhibiter consumption is few, the high and low poison ring of inhibition efficiency is protected, synthesis technique is simple.
the accompanying drawing explanation
embodiment
Below in conjunction with concrete embodiment, the present invention is described in further detail, still, these embodiment are not for limiting the scope of the invention by any way.
The preparation example that embodiment 1～7 is inhibiter;
Embodiment 8～10 is the static corrosion evaluation Example;
Embodiment 11 is high temperature Dynamic Corrosion evaluation Example;
Embodiment 12 is the galvanic corrosion evaluation Example.
Embodiment 1～3 preparation component (A)
Embodiment 1
Oleic acid and diethanolamine are put in reactor according to 1: 2 mol ratio, under constantly stirring, be warming up to 140～220 ℃, pass into N 2gas, reflux 3～6 hours, reduces temperature of reaction to 70～120 ℃, and add the diethanolamine of 1: 2, and add the NaOH of charging capacity 0.5%, and control extent of reaction with acid number, obtain the fatty acid amide intermediate, continue reaction 3～6 hours, after having reacted, intermediate is cooled to below 50 ℃, according to mol ratio 1: 1.1, slowly adds in batches maleic anhydride, 70～110 ℃ of reactions 3～8 hours, obtain amine hydroxybenzene maleic acid ester (A) 1 after cooling after adding.
Embodiment 2
According to preparation method like amine hydroxybenzene maleic acid ester category-A in 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 preparation method like amine hydroxybenzene maleic acid ester category-A in embodiment 1, add the sodium ethylate catalyzer sodium ethylate of charging capacity 0.5% to replace oleic acid by linolic acid, make linolic acid acid amides maleic acid ester (A) 3.
Embodiment 4～6 preparation components (B)
Embodiment 4
Using toluene as solvent, the 0.1mol imidazoles is dissolved in 50mL toluene, then add the diethyl maleate of 0.12mol, reflux 15 hours under 70 ℃, then underpressure distillation, except desolventizing obtains imidazoline ester (B) 1.
Embodiment 5
According to preparing the similar method of imidazoline ester in embodiment 4, replace diethyl maleate by dibutyl maleate, make imidazoline ester (B) 2.
Embodiment 6
According to preparing the similar method of imidazoline ester D in 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 in 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
Figure DEST_PATH_GSB00000498381600031
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 water 2deoxygenation 1h, then pass into CO 2gas 1h until its reach capacity), 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 in Table 2.As can be seen from Table 2, above-mentioned inhibiter is at CO 2all there is corrosion inhibition preferably in corrosive medium.
The static corrosion evaluation of the different inhibiter of table 2
Figure DEST_PATH_GSB00000498381600042
Embodiment 9
Choose HSJ02 in above-described embodiment 7 and, as inhibiter to be evaluated, change the inhibiter consumption, evaluation method is in the same manner as in Example 8, investigates the impact of inhibiter add-on on corrosion inhibition, and experimental result is in Table 3.
The impact of table 3 density of corrosion inhibitor on corrosion inhibition
Figure DEST_PATH_GSB00000498381600043
Figure DEST_PATH_GSB00000498381600051
From table 3, inhibiter is used lower concentration 20～50mg/L just can obtain reasonable corrosion mitigating effect, and this illustrates the anti-CO of this inhibiter 2the excellent property of corrosion.
Embodiment 10
Choose HSJ02 in above-described embodiment 7 and, as inhibiter to be evaluated, change temperature, evaluation method is in the same manner as in Example 8, investigates the impact of temperature on corrosion inhibition, and experimental result is in Table 4.
As can be seen from Table 4, in 30～90 ℃ of scopes, corrosion inhibition rate, all more than 90%, embodies thermal adaptability and stability preferably.
The impact of table 4 temperature on corrosion inhibition
Figure DEST_PATH_GSB00000498381600052
Embodiment 11
Adopt autoclave to carry out CO 2corrosion evaluation test, choose that in above-described embodiment 7, HSJ02 is as the inhibiter of valency to be exposed sb.'s past misdeeds, 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: add 1200mL distilled water in autoclave, hang into test piece except desolventizing, first pass into common N 240min, then pass into high-purity N 240min, and then logical CO 230min, then close intake valve, air outlet valve, and heat temperature raising, after being raised to preset temperature, is opened intake valve, starts pressurising, after being charged to predetermined pressure, closes inlet valve, starts timing.
Test-results is in Table 5, and from table 5, when temperature is 90～130 ℃, with the low-temperature phase ratio, corrosion inhibition rate slightly descends, but still, more than 86%, corrosion mitigating effect is comparatively remarkable, and temperature variation is on its corrosion mitigating effect impact not obvious.
Again in conjunction with the embodiments 10, 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%.
The impact of table 5 temperature on corrosion inhibition
Figure DEST_PATH_GSB00000498381600061
Embodiment 12
Adopt the Autolab electrochemical workstation to carry out the electrochemical measurement of inhibiter.Electrolyzer adopts three-electrode system, and Pt is supporting electrode, and Ag/AgCl is reference electrode, and for working electrode, (area is 0.78cm to cylindrical test piece (20G steel) 2), experimental temperature is 60 ℃, corrosive medium is CO 2saturated solution.It is electrolyzer that experiment adopts six mouthfuls of round-bottomed flasks, and temperature is controlled in water bath with thermostatic control.The working electrode epoxy encapsulation, the working face of the section of only keeping on file is exposed in solution, before test, bottom surface uses respectively 240 *, 400 *, 600 *, 800 * sand papering, use the acetone supersound washing.
During polarization curve is measured, sweep limit is-200～200mv, and sweep velocity is 0.0005V/s; Electrochemical impedance spectroscopy, the sine wave that actuation signal is 5mV, its range of frequency is 1 * 10 5～1 * 10 -2hz, adopt the AutoLab analysis software to carry out data analysis.
The inhibiter HSJ02 chosen in 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 presents high frequency, the double-deck capacitive reactance arc of medium and low frequency.

Claims (8)

1. an inhibiter is characterized in that: composed of the following components: in the inhibiter gross weight:
Figure FSB0000114774810000011
In the inhibiter gross weight, the structural formula of component (A) fatty acid amide maleic acid ester is:
Wherein: R 1for C 10～C 20alkyl or alkenyl,
The structural formula of imidazoline ester is:
Wherein: m=1～4; X=1～3, the positive integer of y=1～3.
2. according to a kind of inhibiter claimed in claim 1, it is characterized in that: the lipid acid in described fatty acid amide is C 15～C 20the monocarboxylic acid of alkyl or alkenyl.
3. according to a kind of inhibiter claimed in claim 1, it is characterized in that: described inhibition auxiliary agent is at least one in thiocarbamide, propiolic alcohol, Sodium dodecylbenzene sulfonate, Sodium orthomolybdate, when the inhibition auxiliary agent is two or more, mixes in any proportion.
4. according to a kind of inhibiter claimed in claim 1, it is characterized in that: described solvent is at least one in water, ethanol, methyl alcohol, Virahol, during both above mixing, mixes in any proportion.
5. according to the preparation method of a kind of inhibiter claimed in claim 1, it is characterized in that, step is as follows:
1) prepare fatty acid amide maleic acid ester (A):
By C 15～C 20the lipid acid of alkyl or alkenyl and diethanolamine drop in reactor according to mol ratio 1:1～1:4, stir and are warming up to 140～220 ℃, pass into N 2gas, reflux 3～6 hours, reduces temperature of reaction to 70～120 ℃, C 15～C 20the lipid acid of alkyl or alkenyl and diethanolamine add the diethanolamine of 1:1～1:4 according to mol ratio, 0.1～2% catalyzer, after the acid number of control product is constant, react 3～6 hours, be cooled to, below 50 ℃, according to mol ratio 1:1～1:2, add maleic anhydride, 70～110 ℃ of reactions 3～8 hours, obtain the fatty acid amide maleic acid ester after cooling;
2) preparation of imidazoline ester:
Take toluene or acetone as solvent, imidazoles is reacted with the unsaturated dibasic acid esters that contains two keys, imidazoles is 1:1～1:2 with the unsaturated dibasic acid esters mol ratio that contains two keys, under 50-90 ℃, refluxes 12～24 hours, except desolventizing obtains imidazoline ester;
3) by step 1) and step 2) 20～80 % by weight (A) and 1～15 % by weight (B) that obtain mixed with the solvent of 1～10 % by weight inhibition auxiliary agent and 5～50 % by weight, obtains inhibiter.
6. according to the preparation method of a kind of inhibiter claimed in claim 5, it is characterized in that: described catalyzer is NaOH, KOH, NaBH 4with any one in sodium ethylate.
7. according to the preparation method of a kind of inhibiter claimed in claim 5, it is characterized in that: described unsaturated dibasic acid esters is diethyl maleate, dibutyl maleate, 5-octene dicarboxylic acid dimethyl ester.
8. according to the application of a kind of inhibiter claimed in claim 1, it is characterized in that: under 30～130 ℃ of conditions, inhibiter is added to and contains CO with the addition of 20～50mg/L 2in the corrosive environment working fluid.
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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 A kind of water-soluble anti-H 2 S inhibiter
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
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
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