CN112341393A - Metal corrosion inhibitor and preparation method thereof - Google Patents
Metal corrosion inhibitor and preparation method thereof Download PDFInfo
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- CN112341393A CN112341393A CN202011243493.3A CN202011243493A CN112341393A CN 112341393 A CN112341393 A CN 112341393A CN 202011243493 A CN202011243493 A CN 202011243493A CN 112341393 A CN112341393 A CN 112341393A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/04—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D233/06—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
- C07D233/08—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms with alkyl radicals, containing more than four carbon atoms, directly attached to ring carbon atoms
- C07D233/12—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms with alkyl radicals, containing more than four carbon atoms, directly attached to ring carbon atoms with substituted hydrocarbon radicals attached to ring nitrogen atoms
- C07D233/16—Radicals substituted by nitrogen atoms
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/14—Nitrogen-containing compounds
- C23F11/149—Heterocyclic compounds containing nitrogen as hetero atom
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D233/00—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings
- C07D233/04—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D233/06—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, directly attached to ring carbon atoms
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/02—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in air or gases by adding vapour phase inhibitors
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/14—Nitrogen-containing compounds
- C23F11/141—Amines; Quaternary ammonium compounds
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/16—Sulfur-containing compounds
Abstract
The invention discloses a metal corrosion inhibitor and a preparation method thereof, comprising a natural gas storage CO2Liquid phase corrosion inhibitor and natural gas storage CO2A gas phase corrosion inhibitor processing step; natural gas storage CO2Preparing a liquid phase corrosion inhibitor: s1, carrying out amidation and cyclization reactions on cis-octadec-9-enoic acid and triethylenetetramine as main components, and carrying out twice dehydration to form an imidazoline intermediate with a five-membered heterocyclic ring; s2, carrying out quaternization on the imidazoline intermediate and benzyl chloride, and converting oil solubility into water-soluble imidazoline quaternary ammonium salt; s3, the imidazoline quaternary ammonium salt reacts with the ethyl sulfur nitrogen, and the ethyl sulfur nitrogen polar group is introduced to enable the imidazoline quaternary ammonium salt to have more active adsorption sitesNatural gas storage CO2The liquid phase corrosion inhibitor is 2-ethionamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt. The invention has the functions of gas-phase corrosion inhibition and liquid-phase corrosion inhibition, and shows that the use concentration of the corrosion inhibitor can be reduced to a lower degree on the premise of not influencing the function of the corrosion inhibitor.
Description
Technical Field
The invention relates to the technical field of protection of natural gas storage, in particular to a metal corrosion inhibitor and a preparation method thereof.
Background
The pressure and the temperature at the bottom of the natural gas storage are high, water usually exists in a steam form, and in the process that natural gas flows from the bottom of the well to the top of the well, the temperature of the natural gas is lower and lower until the temperature is reduced to the dew point of the water, the water in the natural gas can be condensed and gathered on the inner surface of a gas transmission pipeline to form a water film layer. The condensate formed on the pipe wall will gradually accumulate as liquid water in the lower part of the pipeline. A large amount of CO is dissolved in the water film layer on the inner surface of the upper part of the pipeline or the liquid water in the lower part of the pipeline2All cause corrosion to pipelines, i.e. CO is simultaneously present in natural gas gathering pipelines2Gas phase and liquid phase corrosion. CO of traditional liquid phase corrosion inhibitor imidazoline corrosion inhibitor to steel2The corrosion has good liquid phase corrosion inhibition effect, but the vapor pressure of the corrosion is very low, and the corrosion hardly enters the gas phase to inhibit CO in the gas phase2The corrosion of the corrosion inhibitor plays a role in preventing, so that a novel volatile gas-liquid two-phase corrosion inhibitor capable of simultaneously inhibiting corrosion needs to be researched and developed. In the field of metal corrosion inhibitors, research is continuously being carried out to find the desired CO from a large number of novel substances2Corrosion inhibitors, it is desirable that they are effective in controlling and improving the less than perfect quality of the metal corrosion inhibitors. In recent years, various natural gas CO having complicated functions and properties have been proposed by many people2And (4) corrosion inhibitor. In particular to the performances of gas-phase corrosion inhibition, liquid-phase corrosion inhibition, corrosion inhibition speed, economy and the like, and the published technical documents often claim that the corrosion inhibitor with good performances of both gas-phase corrosion inhibition and liquid-phase corrosion inhibition and the like is developed. But so far natural gas CO2Corrosion inhibitor for corrosion preventionThe CO2 gas-liquid two-phase corrosion inhibitor which can simultaneously or simultaneously meet the various performance indexes is not seen.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a metal corrosion inhibitor and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process for preparing the metal corrosion inhibitor includes such steps as using natural gas as gas reservoir to store CO2Liquid phase corrosion inhibitor and natural gas storage CO2A gas phase corrosion inhibitor processing step;
natural gas storage CO2Preparing a liquid phase corrosion inhibitor:
s1, carrying out amidation and cyclization reactions on cis-octadec-9-enoic acid and triethylenetetramine as main components, and carrying out twice dehydration to form an imidazoline intermediate with a five-membered heterocyclic ring;
wherein R is C17H33(ii) a Cis-octadec-9-enoic acid CH3(CH2)7CH＝CH(CH2)7COOH, triethylenetetramine NH2(C2H4NH)2C2H4NH
S2, carrying out quaternization on the imidazoline intermediate and benzyl chloride, and converting oil solubility into water-soluble imidazoline quaternary ammonium salt;
wherein R is C17H33(ii) a R' is C6H5-CH2(ii) a Benzyl chloride C6H5-CH2Cl
S3, imidazoline quaternary ammonium salt reacts with ethyl sulfur nitrogen, and ethyl sulfur nitrogen polar group is introduced to enable imidazoline quaternary ammonium salt to haveNatural gas storage CO with more active adsorption sites2A liquid-phase corrosion inhibitor, namely 2-ethionamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt;
wherein R is C17H33(ii) a R' is C6H5-CH2(ii) a Y is (C)2H5)2NCSS; ethiazathiazide (C)2H5)2NCSSNa table 1 natural gas storage CO2 liquid phase corrosion inhibitor synthesis optimization condition
Natural gas storage CO2Vapor phase corrosion inhibitor
S1, carrying out amidation and cyclization reactions on acetic acid and triethylenetetramine, and dehydrating for two times to form an imidazoline intermediate with five-membered heterocycle;
wherein R is CH3(ii) a Acetic acid CH3COOH
The volatility of the methyl imidazoline intermediate prepared from acetic acid and polyethylene polyamine is obviously improved compared with that of a long-chain imidazoline intermediate with more carbon atoms, and the corrosion prevention of gas-phase CO2 of natural gas is facilitated;
s2, carrying out quaternization on the imidazoline intermediate and benzyl chloride, and converting oil solubility into water-soluble imidazoline quaternary ammonium salt;
wherein R is CH3(ii) a R' is C6H5-CH2
S3, enabling imidazoline quaternary ammonium salt to react with sodium ethyl xanthate, and introducing ethyl xanthate polar groups to enable the imidazoline quaternary ammonium salt to have more active adsorption sites in the CO2 gas phase corrosion inhibitor of the natural gas storage CO2, namely the 2-ethylsulfonic acid aminoethyl benzyl-1-methyl imidazoline quaternary ammonium salt;
wherein R is CH3(ii) a R' is C6H5-CH2(ii) a Y is C2H5An OCSS; ethyl xanthate sodium C2H5OCSSNa。
TABLE 2 optimization conditions for synthesis of CO2 vapor phase corrosion inhibitor for natural gas storage
| Reaction stage | Molar ratio of | Temperature/. degree.C | Reaction time/h |
| Imidazoline synthesis | 1:0.5 (acetic acid: triethylenetetramine) | 220 | 6 |
| Quaternization reaction | 1:2 (imidazoline: benzyl chloride) | 100 | 2.5 |
| Solubilization and synergism reaction | 1:1 (imidazoline Quaternary ammonium salt: sodium ethylxanthate) | 100 | 1 |
Preferably, the cis-octadec-9-enoic acid and triethylene tetramine are dehydrated twice through amidation and cyclization reactions to form a heptadecaimidazoline intermediate with a five-membered heterocycle, and then the heptadecaimidazoline intermediate and benzyl chloride are subjected to quaternization,converting oil solubility into water-soluble imidazoline quaternary ammonium salt; imidazoline quaternary ammonium salt reacts with ethyl sulfur nitrogen, and ethyl sulfur nitrogen polar groups are introduced, so that imidazoline quaternary ammonium salt has natural gas storage CO with more active adsorption sites2The liquid phase corrosion inhibitor is 2-ethionamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt.
Preferably, the acetic acid and the triethylene tetramine are dehydrated twice through amidation and cyclization reactions to form a methyl imidazoline intermediate with five-membered heterocycle, and then the methyl imidazoline intermediate is quaternized with benzyl chloride to be converted from oil solubility into water-soluble imidazoline quaternary ammonium salt; finally, imidazoline quaternary ammonium salt is subjected to substitution reaction with sodium ethylsulfonate, and ethyl sulfonic acid polar group is introduced, so that imidazoline quaternary ammonium salt has more active adsorption sites and natural gas storage CO with higher vapor pressure2The gas phase corrosion inhibitor is 2-ethyl amine sulfonate ethyl benzyl-1-methyl imidazoline quaternary ammonium salt.
A metal corrosion inhibitor, and the natural gas storage CO prepared by the method2The gas-liquid two-phase corrosion inhibitor is formed by compounding a natural gas storage reservoir liquid phase corrosion inhibitor 2-ethylsulfanilamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt and a natural gas storage reservoir gas phase corrosion inhibitor 2-ethylsulfonic acid amidoethylbenzyl-1-methylimidazoline quaternary ammonium salt in a compounding ratio of 1-2: 1, preferably 1.2: 1.
Preferably, the natural gas storage CO2The corrosion inhibitor contains a certain proportion of penetrating foaming agent, and the function of the penetrating foaming agent is to enable injected gas-liquid two-phase CO of the natural gas storage reservoir2The corrosion inhibitor forms a foam state, contacts the inner surface of the pipeline as much as possible under the pushing of natural gas to fully play a gas-liquid two-phase corrosion inhibition role, and the using proportion of the penetrating foaming agent is 0.01-0.1%, preferably 0.02-0.05%.
Preferably, the natural gas storage reservoir is gas-liquid two-phase CO2The corrosion inhibitor can be mixed with other kinds or varieties of CO2The corrosion inhibitor is used in a composite way, and particularly has the best synergistic effect with organic amines such as monoethanolamine, diethanolamine, triethanolamine, N-methyldiethanolamine and cyclohexylamine.
Preferably, the natural gas storage reservoir is gas-liquid two-phase CO2Metal corrosion inhibitors andsodium butylxanthate has a good synergistic corrosion inhibition effect, for example, in the case of N-methyldiethanolamine at a concentration of 40mg/L, monoethanolamine at a concentration of 10mg/L, CO in natural gas reservoirs2When the concentration of the gas-liquid two-phase corrosion inhibitor is 80mg/L, the gas-phase corrosion rate is 0.016mm/a, which is higher than that of the natural gas storage CO added alone2The gas-liquid two-phase corrosion inhibitor has a good performance of 0.019mm/a at a concentration of 130 mg/L.
The natural gas-liquid two-phase carbon dioxide metal corrosion inhibitor provided by the invention has both gas-phase corrosion inhibition and liquid-phase corrosion inhibition functions, and also shows that the use concentration of the corrosion inhibitor can be reduced to a lower degree on the premise of keeping the corrosion inhibitor function unaffected, a layer of compact adsorption film is formed on the metal surface in the gas phase, the utilization rate of the corrosion inhibitor is improved, the adsorption free energy of the corrosion inhibitor on the metal surface and the wetting angle of the metal surface are obviously reduced, the strength and the compactness of the adsorption film formed on the surface of a pipeline in contact with gas are improved, and the purpose of gas-liquid two-phase comprehensive corrosion inhibition.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example one
Preparation of 2-ethionamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt
Amidating cis-octadec-9-enoic acid and triethylenetetramine at a molar ratio of 1:0.55 at 130 ℃ for 1h, cyclizing at 250 ℃ for 7h, adding 2 times of mol of benzyl chloride, quaternizing at 100 ℃ for 3h, and finally adding equimolar ethidene nitrogen at 100 ℃ for reaction for 1h to obtain CO of the natural gas reservoir2The liquid phase corrosion inhibitor in the gas-liquid two-phase corrosion inhibitor is 2-ethionamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt.
Example two
Preparation of 2-ethylxanthate aminoethylbenzyl-1-methylimidazoline quaternary ammonium salt
Amidating acetic acid and triethylenetetramine at the temperature of 120 ℃ for 1h according to the molar ratio of 1:0.5, cyclizing for 6h at the temperature of 220 ℃, adding 2 times of mol of benzyl chloride, carrying out quaternization reaction at the temperature of 100 ℃ for 2.5h, and finally adding equimolar ethyl sulfonate to react for 1h at the temperature of 100 ℃ to obtain the gas phase corrosion inhibitor 2-ethyl sulfonic acid aminoethylbenzyl-1-methylimidazoline quaternary ammonium salt in the gas-liquid two-phase corrosion inhibitor of CO2 of the natural gas reservoir.
EXAMPLE III
Determination of corrosion inhibition rate (liquid phase) by static weightlessness method
The experimental temperature is 50 ℃, the partial pressure of CO2 is 0.50MPa, the degree of mineralization of a liquid phase is 30000mg/L, and CO2Liquid phase corrosion inhibitor 2-ethionamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt (YX), CO2The gas phase corrosion inhibitor 2-ethyl amine sulfonic ethyl benzyl-1-methyl imidazoline quaternary ammonium salt (QX) and the butyl sodium sulfonate (DH) are combined with a liquid phase corrosion inhibition experiment, and the experimental results are shown in a table 3.
TABLE 3 determination of Corrosion inhibition Rate (liquid phase) by static weightlessness method
| concentration/(mg/L) | CR/（mm/a） | IE/% |
| 0 | 0.9214 | —— |
| 150/（QX） | 0.2567 | 72.1 |
| 150（YX） | 0.1516 | 83.5 |
| 150（DH） | 0.4918 | 46.6 |
| 60（QX）+100（YX）+30（DH） | 0.0456 | 95.1 |
Example four
Determination of corrosion inhibition rate (gas phase) by static weightlessness method
Experiment temperature 50 ℃ and CO2Partial pressure of 0.50MPa, liquid phase oreThe chemical degree is 30000mg/L, CO2Liquid phase corrosion inhibitor 2-ethionamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt (YX), CO2The gas phase corrosion inhibitor 2-ethyl amine ethyl benzyl-1-methyl imidazoline quaternary ammonium salt (QX) and the butyl sodium sulfonate (D) are combined to carry out a gas phase corrosion inhibition experiment, and the experimental result is shown in the table 4.
TABLE 4 determination of Corrosion inhibition Rate (gas phase) by static weightlessness method
| concentration/(mg/L) | CR/（mm/a） | IE/% |
| 0 | 0.9473 | —— |
| 100/（QX） | 0.0641 | 93.2 |
| 150（YX） | 0.5529 | 41.6 |
| 150（D） | 0.5819 | 38.6 |
| 70（QX）+50（YX）+20（DH） | 0.0873 | 90.8 |
EXAMPLE five
Determination of corrosion inhibition rate (gas phase) by static weightlessness method
Experiment temperature 50 ℃ and CO2Partial pressure of 0.50MPa, liquid phase mineralization of 30000mg/L, CO2Liquid phase corrosion inhibitor 2-ethionamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt (YX), CO2The gas phase corrosion inhibitor 2-ethyl amine sulfonate ethyl benzyl-1-methyl imidazoline quaternary ammonium salt (QX), N-dimethyl diethanol amine (MDEA) and Monoethanolamine (ME) are combined to carry out gas phase corrosion inhibition experiments, and the experimental results are shown in Table 5.
TABLE 5 determination of Corrosion inhibition Rate (gas phase) by static weightlessness method
| concentration/(mg/L) | CR/（mm/a） | IE/% |
| 0 | 0.9955 | —— |
| 100（MDEA） | 0.3653 | 63.3 |
| 100（MEA） | 0.4531 | 54.5 |
| 30（QX）+30（YX）+100（MDEA）+10（MEA） | 0.0796 | 92.0 |
Natural gas storage CO of the invention in combination with organic amines2The gas-liquid two-phase corrosion inhibitor accounts for the largest proportion, and accounts for 85-100% of the total amount of the compound, preferably 90-100%. The main component is natural gas storage CO in the invention2The gas-liquid two-phase corrosion inhibitor is an important characteristic of the invention. If the natural gas storage reservoir CO of the invention is used as the main component2When the using amount of the gas-liquid two-phase corrosion inhibitor is less than 85 percent, certain problems may occur, most prominently, the gas-liquid two-phase corrosion inhibition rate cannot reach an ideal state, the gas-phase and liquid-phase corrosion inhibition effects cannot be combined, and the using amount of the gas-liquid two-phase corrosion inhibitor in natural gas cannot be effectively reduced2The preferred range of corrosion inhibitor usage is considered to be effective for each function of the respective composite component.
The gas-liquid two-phase CO of the natural gas storage reservoir2The corrosion inhibitor and the sodium butyl xanthate have good corrosion inhibition synergistic effect, the corrosion inhibitor of the invention with the concentration of 100mg/L has obvious influence on the corrosion rate of steel when being compounded with 20 mg/L sodium butyl xanthate. The corrosion rate of the material is particularly obvious in the reduction trend, which shows that the material is butyl yellowThe sodium orthoformate and the gas-liquid two-phase corrosion inhibitor have good synergistic effect; when the concentration of the sodium butyl xanthate is 20 mg/L, the natural gas storage CO of the invention2When the concentration of the gas-liquid two-phase corrosion inhibitor is 100mg/L, the corrosion inhibition efficiency is the best, the corrosion rate is 0.014 mm/a at the lowest, and the corrosion rate is higher than that of the natural gas storage CO which is only added2The gas-liquid two-phase corrosion inhibitor is also good at 150 mg/L, and has ideal corrosion inhibition effect.
CO other than organic amines such as monoethanolamine, diethanolamine, triethanolamine, N-diethanolamine, cyclohexylamine2Corrosion inhibitors, which may have been used for natural gas storage CO2Without especially considering these components as special components of the invention, these CO' s2The corrosion inhibitor can also be mixed with the gas-liquid two-phase CO of the natural gas storage reservoir in the invention2The corrosion inhibitor is used in a compounding way.
As other CO2Specific examples of corrosion inhibitors may be imidazolines: undecylimidazolinyl diquaternary ammonium salts, dodecylimidazoline, 1- (2-aminoethyl) -2-heptylimidazoline, 2-mercaptobenzimidazole, carboxyethylimidazoline, oleamidoimidazoline, thioureidoimidazoline, 1-decyl-3-methylimidazoline ammonium chloride, imidazolinyl asymmetric diquaternary ammonium salts, imidazoline asymmetric phosphate quaternary ammonium salts, thioureidoalkylimidazoline, and the like; organic sulfur species: thiourea, hexanethiol, decanethiol, dodecanethiol, hexadecanethiol, octanethiol, decanethiol, etc.; carboxylic acids: polyaspartic acid, gluconic acid, 11-mercaptoundecanoic acid, 12-aminododecanoic acid, cysteine, glycine, 11-mercaptoundecanoic acid; organic amines and amides: pelargylamine, dodecylamine, hexadecylamine, octadecylamine, 3, 5-dibromo salicylaldehyde-2-thiophenecarboxylhydrazine schiff base, N- (pyridine-2, 6-diyl) bis (1- (4-methyloxyphenyl) -methylamine), polyvinylamine, polyaniline, fatty amide, N- (pyridine-2, 6-diyl) bis (1- (4-methyloxyphenyl) -methylamine), acetamide, thioamide, or the like; quaternary ammonium salts: quaternary ammonium salt of quinoline, dodecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide, hexadecyl trimethyl benzyl ammonium bromide, quaternary ammonium salt of quinoline; polysaccharides: glycolipid, polysaccharide lipid, lipopeptide, neutral lipid derivative, sophorolipid, and valeric acid-m-diallyl glucoseGlucose and the like; surfactants: tween 80, Tween20, Span20, Span80, hydroxyl gemini surfactant, alkylphenol ethoxylate, fatty alcohol polyoxyethylene ether, cocamide polyoxyethylene ether and the like; others such as caffeine, nicotine, 4-vinylpiperidine, sodium benzoate, 2-methylimidazole, and the like.
The invention selects fatty acid and polyamine as raw materials, and adopts a vacuum method to synthesize imidazoline compounds with different carbon contents. Synthesizing a cyclic imidazoline intermediate through amidation and cyclization processes, performing water-solubility modification on the cyclic imidazoline intermediate by using a quaternizing agent, and introducing ethidium nitrogen and an ethylxanthic acid group to further enhance the water solubility and introduce a plurality of active centers.
Natural gas storage CO as production of the invention2The fatty acid of the gas-liquid two-phase corrosion inhibitor can be various saturated or unsaturated fatty acids with different carbon atoms, but the corrosion inhibition rate and the gas-liquid phase corrosion environment are comprehensively considered, and the natural gas storage CO gas storage tank disclosed by the invention2The liquid phase corrosion inhibitor in the gas-liquid two-phase corrosion inhibitor adopts cis-octadec-9-enoic acid with longer carbon chain; in contrast to liquid phase corrosion inhibitors, which should have suitable volatility in order to be able to be present in sufficient concentration in natural gas, acetic acid with a lower carbon number is used as the acid component.
The polyamine in the raw material for preparing the gas-liquid two-phase corrosion inhibitor for the natural gas storage CO2 can be various unsaturated polyamines with different carbon atom numbers, but the corrosion inhibition rate, the production conditions and the easy availability of the raw material are comprehensively considered, so that the CO2 gas-liquid two-phase corrosion inhibitor for the natural gas storage can be prepared2The liquid phase inhibitor and the gas phase inhibitor in the gas-liquid two-phase inhibitor both adopt triethylenetetramine.
Production of natural gas reservoir CO of the invention from fatty acids and triethylenetetramine2The gas-liquid two-phase corrosion inhibitor, especially the liquid phase corrosion inhibitor, is difficult to dissolve in water and difficult to exert the corrosion inhibition performance due to the existence of longer carbon chain hydrophobic groups. The key to solving the problem is how to improve the water solubility and stability of the imidazoline product on the basis of not changing the excellent corrosion inhibition effect of the imidazoline product, and the invention adopts a benzyl chloride quaternization method. Imidazoline water removal after quaternizationBesides the solubility is improved to a certain extent, the large pi bond of the benzyl benzene also has stronger electron donating capability, and the chemical adsorption center of the corrosion inhibitor and the metal atom can be increased, so that the formed film is more compact and tougher.
Natural gas storage CO synthesized by cis-octadec-9-enoic acid, acetic acid, triethylene tetramine and benzyl chloride2Although the water solubility of imidazoline is improved to a great extent by two imidazoline quaternary ammonium salts of the gas-liquid two-phase corrosion inhibitor, the product, especially the liquid phase corrosion inhibitor, is still too viscous to be used, and needs to be further modified. The natural gas storage CO of the invention2The modifier of the liquid phase corrosion inhibitor in the gas-liquid two-phase corrosion inhibitor adopts ethion-nitrogen, namely, the equimolar ethion-nitrogen is added into the quaternary ammonium salt product of the liquid phase corrosion inhibitor, and a polar group of the ethion-nitrogen is introduced by constant temperature reaction to further enhance the water solubility of the liquid phase corrosion inhibitor and introduce a plurality of active centers to obtain CO of the natural gas storage2The liquid phase corrosion inhibitor is 2-ethionamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt. The natural gas storage CO of the invention2The gas phase corrosion inhibitor modifier in the gas-liquid two-phase corrosion inhibitor is sodium ethyl xanthate, namely, the gas phase corrosion inhibitor quaternary ammonium salt product is added with the equal molar sodium ethyl xanthate, the ethyl xanthate is introduced through constant temperature reaction, the water solubility of the gas phase corrosion inhibitor quaternary ammonium salt product is further enhanced, and a plurality of active centers are introduced in the industry to obtain the CO of the natural gas storage reservoir2The gas phase corrosion inhibitor is 2-ethyl amine sulfonate ethyl benzyl-1-methyl imidazoline quaternary ammonium salt.
The natural gas storage CO of the invention2Although the gas-liquid two-phase corrosion inhibitor has better corrosion inhibition effect, the gas-liquid two-phase corrosion inhibitor has the limitation on CO in gas phase due to the action of gravity and volatility2The corrosion prevention effect of (A) is still slightly insufficient, and compact CO cannot be formed on the metal surface in the gas phase well2The isolation diaphragm limits the use of the isolation diaphragm in metal pipeline transportation of natural gas, thereby being suitable for the pipeline transportation of natural gas. Addition of penetrating foaming agent to CO in natural gas storage reservoir2The gas-phase corrosion inhibition performance of the gas-liquid two-phase corrosion inhibitor has great influence, and the foaming agent can promote the CO in the natural gas storage reservoir2The gas-liquid two-phase corrosion inhibitor forms moderate foam and is carried in the pipeline by natural gasRadial movement forms a layer of compact adsorption film on the metal surface in the gas phase, thus improving the utilization rate of the corrosion inhibitor. The permeable foaming agent also has stronger permeability, and can obviously improve the CO content of the natural gas storage reservoir2The activation capability of the gas-liquid two-phase corrosion inhibitor obviously reduces the adsorption free energy of the corrosion inhibitor on the metal surface and the wetting angle of the metal surface, so that the strength and the compactness of an adsorption film formed on the surface of a pipeline in contact with gas are improved, and the aim of comprehensively inhibiting gas-liquid two-phase corrosion is fulfilled.
It is contemplated that any one of surfactants including anionic surfactants, cationic surfactants, nonionic surfactants, amphoteric surfactants, and polymeric surfactants may be used.
Specific examples of the anionic surfactants which can be effectively used are alkyl sulfate salts such as sodium lauryl sulfate, potassium lauryl sulfate, ammonium lauryl sulfate; alkyl sulfonates such as sodium dodecylbenzenesulfonate, sodium tetradecylbenzenesulfonate, sodium higher alkylnaphthalenesulfonate; fatty acid salts such as sodium laurate, sodium oleate, and sodium linoleate.
Examples of nonionic surfactants are sorbitan fatty acid esters, alkylphenol ethoxylates, fatty alcohol ethoxylates, polyethers.
Examples of such polymeric surfactants include polyvinyl alcohol, polyvinylpyrrolidone and polyethylene glycol, which also function as protective colloids.
When the above-mentioned foaming agent is used, it is only required to be used in an amount such that it exhibits an action capable of promoting foam formation and appropriate stabilization. Therefore, the amount thereof is usually 0.01% to 0.1%, preferably 0.02% to 0.05%, based on the total amount of the corrosion inhibitor component. If less than 0.01% of the penetrating foaming agent is used, this may result in a loss of stability of the foam formed and failure to achieve the gas phase corrosion inhibition objective. On the contrary, if the amount exceeds 0.1%, the excess portion is liable to cause a large amount of foam to form vapor lock to natural gas and unnecessary cost consumption.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. The preparation method of the metal corrosion inhibitor is characterized by comprising the steps of preparing natural gas storage CO2Liquid phase corrosion inhibitor and natural gas storage CO2A gas phase corrosion inhibitor processing step;
natural gas storage CO2Preparing a liquid phase corrosion inhibitor:
s1, carrying out amidation and cyclization reactions on cis-octadec-9-enoic acid and triethylenetetramine as main components, and carrying out twice dehydration to form an imidazoline intermediate with a five-membered heterocyclic ring;
wherein R is C17H33(ii) a Cis-octadec-9-enoic acid CH3(CH2)7CH＝CH(CH2)7COOH, triethylenetetramine NH2(C2H4NH)2C2H4NH
S2, carrying out quaternization on the imidazoline intermediate and benzyl chloride, and converting oil solubility into water-soluble imidazoline quaternary ammonium salt;
wherein R is C17H33(ii) a R' is C6H5-CH2(ii) a Benzyl chloride C6H5-CH2Cl
S3, enabling imidazoline quaternary ammonium salt to react with ethyl sulfur nitrogen, introducing ethyl sulfur nitrogen polar groups, and enabling imidazoline quaternary ammonium salt to have natural gas storage CO with more active adsorption sites2Liquid phase corrosion inhibitor 2-ethylsulfanylaminoethylBenzyl-1-heptadecenyl imidazoline quaternary ammonium salt;
wherein R is C17H33(ii) a R' is C6H5-CH2(ii) a Y is (C)2H5)2NCSS; ethiazathiazide (C)2H5)2NCSSNa
TABLE 1 optimization conditions for synthesis of CO2 liquid phase corrosion inhibitor for natural gas storage
Natural gas storage CO2Vapor phase corrosion inhibitor
S1, carrying out amidation and cyclization reactions on acetic acid and triethylenetetramine, and dehydrating for two times to form an imidazoline intermediate with five-membered heterocycle;
wherein R is CH3(ii) a Acetic acid CH3COOH
The volatility of the methyl imidazoline intermediate prepared from acetic acid and polyethylene polyamine is obviously improved compared with that of a long-chain imidazoline intermediate with more carbon atoms, and the corrosion prevention of gas-phase CO2 of natural gas is facilitated;
s2, carrying out quaternization on the imidazoline intermediate and benzyl chloride, and converting oil solubility into water-soluble imidazoline quaternary ammonium salt;
wherein R is CH3(ii) a R' is C6H5-CH2
S3, enabling imidazoline quaternary ammonium salt to react with sodium ethyl xanthate, and introducing ethyl xanthate polar groups to enable the imidazoline quaternary ammonium salt to have more active adsorption sites in the CO2 gas phase corrosion inhibitor of the natural gas storage CO2, namely the 2-ethylsulfonic acid aminoethyl benzyl-1-methyl imidazoline quaternary ammonium salt;
wherein R is CH3(ii) a R' is C6H5-CH2(ii) a Y is C2H5An OCSS; ethyl xanthate sodium C2H5OCSSNa
TABLE 2 optimization conditions for synthesis of CO2 vapor phase corrosion inhibitor for natural gas storage
2. The preparation method of the metal corrosion inhibitor according to claim 1, wherein cis-octadec-9-enoic acid and triethylenetetramine are subjected to amidation and cyclization reactions for two times to dehydrate to form a heptadecaimidazoline intermediate with a five-membered heterocycle, and then are subjected to quaternization with benzyl chloride to convert oil solubility into water-soluble imidazoline quaternary ammonium salt; imidazoline quaternary ammonium salt reacts with ethyl sulfur nitrogen, and ethyl sulfur nitrogen polar groups are introduced, so that imidazoline quaternary ammonium salt has natural gas storage CO with more active adsorption sites2The liquid phase corrosion inhibitor is 2-ethionamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt.
3. The preparation method of the metal corrosion inhibitor according to claim 1, wherein acetic acid and triethylenetetramine are dehydrated twice through amidation and cyclization reactions to form a methyl imidazoline intermediate with five-membered heterocycle, and then the methyl imidazoline intermediate is converted into water-soluble imidazoline quaternary ammonium salt from oil solubility through quaternization with benzyl chloride; last microphoneThe oxazoline quaternary ammonium salt and sodium ethyl sulfonate are subjected to substitution reaction, and ethyl sulfonic acid polar groups are introduced, so that the imidazoline quaternary ammonium salt has more active adsorption sites and natural gas storage CO with higher vapor pressure2The gas phase corrosion inhibitor is 2-ethyl amine sulfonate ethyl benzyl-1-methyl imidazoline quaternary ammonium salt.
4. The metal corrosion inhibitor is characterized in that the natural gas storage CO prepared by the method2The gas-liquid two-phase corrosion inhibitor is formed by compounding a natural gas storage reservoir liquid phase corrosion inhibitor 2-ethylsulfanilamidoethylbenzyl-1-heptadecenyl imidazoline quaternary ammonium salt and a natural gas storage reservoir gas phase corrosion inhibitor 2-ethylsulfonic acid amidoethylbenzyl-1-methylimidazoline quaternary ammonium salt in a compounding ratio of 1-2: 1, preferably 1.2: 1.
5. The metal corrosion inhibitor of claim 4, wherein the natural gas storage CO is a natural gas storage CO2The corrosion inhibitor contains a certain proportion of penetrating foaming agent, and the function of the penetrating foaming agent is to enable injected gas-liquid two-phase CO of the natural gas storage reservoir2The corrosion inhibitor forms a foam state, contacts the inner surface of the pipeline as much as possible under the pushing of natural gas to fully play a gas-liquid two-phase corrosion inhibition role, and the using proportion of the penetrating foaming agent is 0.01-0.1%, preferably 0.02-0.05%.
6. The metal corrosion inhibitor of claim 4, wherein the natural gas storage reservoir gas-liquid two-phase CO2The corrosion inhibitor can be mixed with other kinds or varieties of CO2The corrosion inhibitor is used in a composite way, and particularly has the best synergistic effect with organic amines such as monoethanolamine, diethanolamine, triethanolamine, N-methyldiethanolamine and cyclohexylamine.
7. The metal corrosion inhibitor of claim 4, wherein the natural gas storage reservoir gas-liquid two-phase CO2The metal corrosion inhibitor and the sodium butyl xanthate have good synergistic corrosion inhibition effect, for example, the concentration of N-methyldiethanolamine is 40mg/L, the concentration of monoethanolamine is 10mg/L, and CO in a natural gas storage reservoir2Gas-liquid two-phaseWhen the concentration of the corrosion inhibitor is 80mg/L, the gas phase corrosion rate is 0.016mm/a, which is higher than that of the natural gas storage CO added alone2The gas-liquid two-phase corrosion inhibitor has a good performance of 0.019mm/a at a concentration of 130 mg/L.
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