CN113278409B - High-temperature acidizing corrosion inhibitor - Google Patents
High-temperature acidizing corrosion inhibitor Download PDFInfo
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- CN113278409B CN113278409B CN202110692034.1A CN202110692034A CN113278409B CN 113278409 B CN113278409 B CN 113278409B CN 202110692034 A CN202110692034 A CN 202110692034A CN 113278409 B CN113278409 B CN 113278409B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/72—Eroding chemicals, e.g. acids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D401/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
- C07D401/02—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
- C07D401/12—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings linked by a chain containing hetero atoms as chain links
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D513/00—Heterocyclic compounds containing in the condensed system at least one hetero ring having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for in groups C07D463/00, C07D477/00 or C07D499/00 - C07D507/00
- C07D513/02—Heterocyclic compounds containing in the condensed system at least one hetero ring having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for in groups C07D463/00, C07D477/00 or C07D499/00 - C07D507/00 in which the condensed system contains two hetero rings
- C07D513/04—Ortho-condensed systems
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/32—Anticorrosion additives
Abstract
The invention discloses a high-temperature acidizing corrosion inhibitor, belonging to the technical field of oil and gas field exploitation corrosion prevention. The mass ratio of the corrosion inhibition main agent to the auxiliary agent A to the auxiliary agent B is 10:3: 1. The corrosion inhibitor is formed by mixing a main corrosion inhibitor, an auxiliary agent A and an auxiliary agent B, and is dissolved into a corrosion inhibitor solution by using ethanol when in use. The preparation method of the main corrosion inhibitor comprises the following steps: cyanoguanidine, 4- (((4-chloropyridin-2-yl) oxy) methyl) benzonitrile and potassium hydroxide are reacted in a solvent ethylene glycol monoethyl ether at 120 ℃ for 2 hours to generate a product 6- (4- (((4-chloropyridin-2-yl) oxy) methyl) benzonitrile) 1,3, 5-triazine-2, 4, diamine, namely the main corrosion inhibitor. The auxiliary agent B is prepared by reacting raw materials of N, N-dimethylamine and oxalic acid at 90 ℃ for 6 hours in the presence of a catalyst. The corrosion inhibitor has the advantages of good solubility, more adsorption sites, high corrosion inhibition efficiency, low toxicity and the like in a high-temperature acidification environment.
Description
Technical Field
The invention relates to the technical field of oil and gas field exploitation anticorrosion, in particular to a novel environment-friendly high-temperature acidizing corrosion inhibitor.
Background
As an important means for improving the single-well productivity of the oil-gas well, the acidizing operation can still be applied in large scale in the development of deep and ultra-deep oil-gas reservoirs, but under the conditions of high temperature and high acid solution concentration (hydrochloric acid concentration is 20%), the corrosion risk of the acid solution to the underground pipe column can be greatly improved, and the most common solution is to add a corrosion inhibitor.
Corrosion inhibitors, also known as corrosion inhibitors, are chemicals or compounds that are present in the environment (medium) in appropriate concentrations and forms to prevent or slow down the corrosion of materials. The corrosion inhibitor has the characteristics of low cost, simple operation, quick response, suitability for long-term use and the like. As an economic, effective and strong-universality metal corrosion control method, the method is one of the most common protective measures in an oil field system. A great deal of work is done on the aspects of developing and researching the acidizing corrosion inhibitor at home and abroad, but reports on the high-performance acidizing corrosion inhibitor suitable for high-temperature concentrated acid are few, and the common acidizing corrosion inhibitor still has the defects of low corrosion inhibition efficiency, poor compatibility, easiness in precipitation, easiness in layering and the like in practical application, so that the requirement on underground pipe column corrosion protection under severe acidizing conditions is difficult to effectively meet. And most of the high-temperature acidizing corrosion inhibitors used in the field of oil reservoir modification at present have the defects of poor solubility, easy coking and the like, and the commonly used compound high-temperature acidizing corrosion inhibitors are mainly alkynol corrosion inhibitors, and although the corrosion resistance of products is greatly improved by alkynol substances, the acetylene alcohol corrosion inhibitors have the defects of high price, high toxicity and the like. Therefore, the research on improving the performance index of the acidizing corrosion inhibitor is particularly important for realizing effective corrosion prevention of equipment such as underground pipelines and the like.
Disclosure of Invention
The invention aims to provide a corrosion inhibitor in a high-temperature acidification environment, aiming at the defects of the existing corrosion inhibitor in the high-temperature acidification environment.
The high-temperature acidification corrosion inhibitor provided by the invention consists of a main corrosion inhibition agent, an auxiliary agent A and an auxiliary agent B. The mass ratio of the corrosion inhibition main agent to the auxiliary agent A to the auxiliary agent B is 10:3: 1. The corrosion inhibitor is formed by mixing a main corrosion inhibitor, an auxiliary agent A and an auxiliary agent B, and is dissolved into a corrosion inhibitor solution by using ethanol when in use.
The preparation method of the corrosion inhibition main agent comprises the following steps: cyanoguanidine, 4- (((4-chloropyridin-2-yl) oxy) methyl) benzonitrile and potassium hydroxide are reacted in a solvent ethylene glycol monoethyl ether at 120 ℃ for 2 hours to generate a product 6- (4- (((4-chloropyridin-2-yl) oxy) methyl) benzonitrile) 1,3, 5-triazine-2, 4, diamine, namely the main corrosion inhibitor. The molecular structural formula of the main corrosion inhibitor is as follows:
the preparation method of the auxiliary agent A comprises the following steps: halogenated alpha-amino ketone and thiocarbohydrazide are subjected to condensation reaction for 1H at the temperature of 150 ℃ to generate an intermediate 1, the intermediate 1 is subjected to oxidation reaction of sodium nitrite to generate an intermediate 2, and the intermediate 2 is subjected to coupling reaction in the excess hydrochloric acid to generate 6-amino-7H-tetrazolo [5, 1-b ] [1, 3, 4] -thiadiazine, namely the auxiliary agent A. The molecular structural formula of the auxiliary agent A is as follows:
the adjuvant B is used as a high-temperature synergist. The auxiliary agent B is prepared by reacting raw materials of N, N-dimethylamine and oxalic acid for 6 hours at the temperature of 90 ℃ in the presence of a catalyst CGP-1. The mol ratio of the N, N-dimethylamine to the oxalic acid to the catalyst is 2: 6: 3.
The high-temperature synergist enhances the corrosion inhibition effect through the synergistic effect with the main corrosion inhibition agent, changes the physical state or chemical bond of the surface of the steel sheet, forms a complex with part of the main corrosion inhibition agent through the hydrolysis effect under high-temperature and acidic conditions, further enhances the adsorption effect of the corrosion inhibitor on the iron surface, and can fill the gaps of a macromolecular corrosion inhibitor film because the high-temperature synergist is a micromolecule, so that the film is more compact, and the corrosion inhibition effect under the high-temperature condition is improved.
The principle that the corrosion inhibitor is adsorbed on the metal surface to form a corrosion inhibitor film so as to achieve the corrosion inhibition effect is as follows:
(1) compared with physical adsorption, the chemical adsorption force is stronger, so that the force of most organic corrosion inhibitors on metal surfaces is mainly realized through chemical adsorption, and the chemical adsorption is essentially that coordination bonds are formed between corrosion inhibitor molecules or ions and metal surface atoms.
(2) According to the extra-nuclear electron arrangement of iron atoms, the empty d orbitals exist on the surfaces of the iron atoms, and atoms such as N, O, S, P contained in the corrosion inhibitor have lone pair electrons, so that coordination bonds can be formed with the d orbitals of the iron atoms, molecules or ions of the corrosion inhibitor are firmly adsorbed on the metal surfaces through the strong action force of the chemical bonds such as the coordination bonds, and the adsorption is called chemical adsorption.
(3) For unsaturated molecules such as double bonds, triple bonds or benzene rings with conjugated structures, the conjugation enables electron clouds to be distributed on the conjugated structures in a dispersing mode, the electrons can also be dispersed to empty d orbitals on the metal surface to form coordinate bonds, namely pi bond adsorption, and the adsorption is greatly influenced by a steric hindrance effect. In addition, when the unsaturated bond is adjacent to the polar group, conjugation can be formed between the unsaturated bond and the polar group, the electron cloud density is improved, the unsaturated bond is adsorbed on the metal surface in a planar structure, the corrosion inhibition effect of the corrosion inhibitor can be improved, and the compound containing the benzene ring belongs to a typical pi bond adsorption type corrosion inhibitor.
Compared with the prior art, the invention has the advantages that:
the corrosion inhibitor is suitable for severe working conditions of high-temperature deep well acidification construction, and improves the high-temperature corrosion inhibition comprehensive performance of the corrosion inhibitor. The corrosion inhibition main agent molecules form coordination bonds with metal atoms through active neutral N, O, S heteroatoms, large pi bonds of benzene rings and the like, and simultaneously are accompanied with feedback bond action and physical adsorption to form a main agent molecule adsorption film, so that more adsorption sites can be provided. The auxiliary agent A and the auxiliary agent B (high-temperature synergist) belong to small molecular structures, and at the moment, a small-area adsorption film is constructed in the pores of a corrosion inhibition main agent molecular adsorption film or on the metal surface where the main agent molecular film cannot be constructed, so that the compactness of the corrosion inhibitor film is enhanced, and the corrosion of high-temperature acid liquor to metal is inhibited by the synergy of the corrosion inhibitor film and the main agent molecules. And the corrosion inhibitor has the characteristics of environmental protection and no toxicity.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and description, and is in no way intended to limit the invention.
Example 1
The reaction formula for preparing the main agent of the corrosion inhibitor is as follows:
the preparation method of the main agent of the corrosion inhibitor comprises the following steps:
2.53mmol of cyanoguanidine, 2.25mmol of 4- (((4-chloropyridin-2-yl) oxy) methyl) benzonitrile and 2.53mmol of potassium hydroxide are put into a flask and mixed uniformly, 80ml of ethylene glycol monoethyl ether is added as a solvent, the mixture is heated to 120 ℃ and reacted for 2 hours at constant temperature, then petroleum ether is used for extraction and purification, and the mixture is put into a vacuum drying oven for drying to finally obtain a main product 6- (4- (((4-chloropyridin-2-yl) oxy) methyl) benzonitrile) 1,3, 5-triazine-2, 4, diamine.
Example 2
The preparation method of the auxiliary agent A of the corrosion inhibitor comprises the following steps:
the method mainly adopts a one-pot method, 1mol of chloro alpha-aminoketone and 1.1mol of thiocarbohydrazide are subjected to simple condensation reaction for 1 hour at the temperature of 150 ℃ to generate an intermediate 1, then 2mol of sodium nitrite is added and fully stirred to generate oxidation reaction for 1.5 hours to generate an intermediate 2, then 2mol of hydrochloric acid is added and fully stirred to generate intramolecular coupling reaction for 1.5 hours, the reaction is cooled to room temperature, reduced pressure distillation, washing, filtering and drying are carried out, and finally the product 6-amino-7H-tetrazolo [5, 1-b ] [1, 3, 4] -thiadiazine, namely the auxiliary agent A, is obtained. The reaction process is as follows:
example 3
The preparation method of the auxiliary agent B (high-temperature synergist) of the corrosion inhibitor comprises the following steps:
the high-temperature synergist is prepared by taking N, N-dimethylamine, oxalic acid and a CGP-1 catalyst as raw materials, and the synthesis conditions are as follows: the molar ratio of the N, N-dimethylamine, the oxalic acid and the CGP-1 catalyst is 2: 6: 3, the reaction temperature is 90 ℃, and the reaction time is 6 hours, so that an auxiliary agent B is obtained.
Test and test:
the corrosion inhibitor is prepared by uniformly mixing the three corrosion inhibitor components prepared in the examples 1, 2 and 3 according to the mass ratio of 10:3:1 of the main corrosion inhibitor, the auxiliary A and the auxiliary B. After weighing the corrosion inhibitor, adding the corrosion inhibitor into the experimental solution after completely dissolving the corrosion inhibitor by using enough ethanol.
And (3) carrying out a corrosion weight loss test on the N80 steel by adopting a rotary hanging piece method, wherein the rotation speed is 60 r/min. The base solution of the test solution was a 3.5% NaCl solution. Different acid solutions were added to the NaCl solution to simulate the corrosive solution. The test is carried out in a high-temperature autoclave under different temperature and pressure conditions for 4 h. Each coupon was weighed accurately to the nearest 0.0001g before the test began. And (4) taking out the hanging piece after the test, and recording the surface state of the hanging piece and the distribution of corrosion products. Cleaning the hanging sheet by using 10% triammonium citrate, cleaning the hanging sheet by using acetone and absolute ethyl alcohol one by one, placing the hanging sheet on clean filter paper, finally drying the hanging sheet by using cold air, placing the hanging sheet in a dryer for drying for 20min, weighing the hanging sheet, and accurately weighing the hanging sheet to 0.0001 g. And calculating the corrosion rate and the corrosion inhibition efficiency according to the mass difference before and after corrosion. The control of the test conditions and the test results are shown in Table 1. In table 1, the mass fraction of the corrosion inhibitor refers to the mass percentage of the total mass of the main corrosion inhibitor, the auxiliary agent a and the auxiliary agent B in the corrosive solution.
TABLE 1 control of test conditions and test result data
The data in the table show that the corrosion inhibitor of the invention shows obvious corrosion inhibition effect under the high-temperature condition of high-concentration acid, and proves that the corrosion inhibitor is suitable for metal corrosion prevention under the high-temperature and high-acid environment, and is a novel environment-friendly high-temperature acidification corrosion inhibitor.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. The high-temperature acidizing corrosion inhibitor is characterized by comprising a main corrosion inhibitor, an auxiliary agent A and an auxiliary agent B; the molecular structural formula of the main corrosion inhibition agent is as follows:
the preparation method of the corrosion inhibition main agent comprises the following steps: putting cyanoguanidine, 4- (((4-chloropyridin-2-yl) oxy) methyl) benzonitrile and potassium hydroxide into a flask, uniformly mixing, adding ethylene glycol monoethyl ether as a solvent, heating to 120 ℃, reacting at constant temperature for 2 hours, extracting and purifying by using petroleum ether, and drying in a vacuum drying oven to obtain a main product 6- (4- (((4-chloropyridin-2-yl) oxy) methyl) benzonitrile) 1,3, 5-triazine-2, 4, diamine;
the molecular structural formula of the auxiliary agent A is as follows:
the adjuvant B is a high-temperature synergist.
2. The high-temperature acidizing corrosion inhibitor as claimed in claim 1, wherein the auxiliary agent B is prepared by reacting raw materials of N, N-dimethylamine and oxalic acid in the presence of a catalyst CGP-1 at the temperature of 90 ℃ for 6 hours.
3. The high temperature acidizing corrosion inhibitor of claim 2 wherein the molar ratio of N, N-dimethylamine, oxalic acid, catalyst CGP-1 is 2: 6: 3.
4. The high-temperature acidification corrosion inhibitor as claimed in claim 1, wherein the mass ratio of the main corrosion inhibitor, the auxiliary agent A and the auxiliary agent B is 10:3: 1.
5. A high temperature acidizing corrosion inhibitor according to claim 4 wherein the corrosion inhibitor is formed by mixing the main corrosion inhibitor, the auxiliary agent A and the auxiliary agent B and is dissolved in ethanol to form a corrosion inhibitor solution when in use.
6. The high temperature acidizing corrosion inhibitor of claim 1 wherein said adjuvant a is prepared by the process of: halogenated alpha-amino ketone and thiocarbohydrazide are subjected to condensation reaction for 1H at the temperature of 150 ℃ to generate an intermediate 1, the intermediate 1 is subjected to oxidation reaction of sodium nitrite to generate an intermediate 2, and the intermediate 2 is subjected to coupling reaction in the excess hydrochloric acid to generate 6-amino-7H-tetrazolo [5, 1-b ] [1, 3, 4] -thiadiazine, namely the auxiliary agent A.
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