A preparation method of metal corrosion inhibition component and its product and application

Abstract

The present invention discloses a method for preparing a metal corrosion inhibitor component, its products, and applications. The method involves reacting a halogenated tetraphenylethylene with aminopolyethylene glycol or aminoethanol to produce a metal corrosion inhibitor component. The component exhibits excellent corrosion inhibition performance and is easily detectable in corrosive media. Furthermore, the component emits strong fluorescence upon adsorption onto metal surfaces, enabling visual detection.

Description

Technical Field

[0001] The present invention relates to a preparation method of a metal corrosion inhibition component, a product thereof and an application thereof, and in particular to a preparation method of a metal corrosion inhibition component with a fluorescence effect, a product thereof and an application thereof. Background Art

[0002] Metal corrosion is a widespread problem in industrial production. Safety accidents and unplanned shutdowns caused by metal corrosion cause significant losses to companies. For example, during oil and gas field development, fracturing and acidizing processes, oil wells, tubing, casing, sucker rods, and pipelines, equipment, and containers in surface gathering and transportation systems often suffer from severe corrosion. This not only causes equipment scrapping and replacement, requiring shutdowns for maintenance, but also leads to oil and gas leaks and environmental pollution. Metal corrosion prevention measures include material upgrades, process corrosion prevention, and corrosion monitoring. Corrosion monitoring is the foundation for predictive maintenance and effective process corrosion prevention.

[0003] Upgrading metal materials and choosing more corrosion-resistant metal materials is one way to slow down corrosion, but adding metal corrosion inhibitors is more economical. Common metal corrosion inhibitors include organic amines, thiourea derivatives, imidazoline derivatives, acetylene alcohols, benzotriazoles, etc., but these metal corrosion inhibitors each have shortcomings, such as unsatisfactory corrosion inhibition performance and poor water solubility. Therefore, it is necessary to provide new corrosion inhibitors with better performance. The effective concentration of existing metal corrosion inhibitors is not easy to detect, and it is difficult to implement more targeted replenishment measures. The current method is to periodically add corrosion inhibitors in a quantitative manner, which makes it difficult to ensure the appropriate dosage of the agent. When the concentration of the agent is too high, it will be wasted, and when it is too low, the required corrosion inhibition effect will not be achieved. In particular, it is even more difficult to detect the degree of adsorption of existing metal corrosion inhibitors on the metal surface, and predictive positioning maintenance and repair cannot be achieved.

[0004] The information disclosed in the foregoing background section is only for enhancement of understanding of the background of the invention and may include information that is not known to one of ordinary skill in the art. Summary of the Invention

[0005] The purpose of the present invention is to provide a method for preparing a metal corrosion inhibition component. On the basis of achieving the above-mentioned purpose, the present invention also provides a metal corrosion inhibition method and a corrosion protection method using the product thereof.

[0006] The main contents of the present invention are as follows:

[0007] 1. A method for preparing a metal corrosion inhibition component, comprising: reacting a compound represented by formula I with a compound represented by formula II in the presence of copper powder in a solvent-free or organic solvent;

[0008]

[0009] wherein R1′, R2′ and R3′ are each independently a hydrogen atom, a hydrocarbon group or the same as X, X is —Cl, —Br or —I; and n is 0 to 50.

[0010] 2. A preparation method according to any of the above, characterized in that, in the compound represented by formula II, n is 0-30, preferably 0-16, and more preferably 0-12.

[0011] 3. A preparation method according to any of the above, characterized in that, in the compound represented by formula I, the substituents on the benzene ring (marked as ①, ②, ③, ④) are all located in the para position of the vinyl group.

[0012] 4. The preparation method according to any of the foregoing, characterized in that one of R1', R2' and R3' is the same as X, and the remaining substituents are each independently a hydrogen atom or a hydrocarbon group; or two of R1', R2' and R3' are the same as X, and the other substituent is a hydrogen atom or a hydrocarbon group; or R1', R2' and R3' are all the same as X.

[0013] 5. A preparation method according to any of the above, characterized in that the molar ratio of the compound of formula I, copper and the compound of formula II is 1:(0.01-1):(1-100), preferably 1:(0.03-0.5):(3-30).

[0014] 6. A preparation method according to any of the above, characterized in that the reaction temperature is 80°C to 200°C.

[0015] 7. A preparation method according to any of the above, characterized in that the reaction time is 2h to 168h.

[0016] 8. A preparation method according to any of the above, characterized in that the reaction solvent is 1,4-dioxane, N,N'-dimethylformamide, N,N'-dimethylacetamide, dimethyl sulfoxide or N-methylpyrrolidone.

[0017] 9. A metal corrosion inhibition component, characterized in that it is prepared by any of the above methods.

[0018] 10. Application of the aforementioned metal corrosion inhibition components in metal hydrogen evolution corrosion protection.

[0019] 11. A metal corrosion inhibitor, characterized by comprising the metal corrosion inhibition component described in 9.

[0020] 12. A metal corrosion inhibition method, characterized in that the corrosive medium contains the metal corrosion inhibition component described in 9.

[0021] 13. A metal corrosion inhibition method, characterized in that the corrosive medium contains the metal corrosion inhibition component described in 9, and the concentration of the metal corrosion inhibition component in the corrosive medium is detected and controlled by ultraviolet-visible absorption spectroscopy; preferably, the concentration of the metal corrosion inhibition component in the corrosive medium is controlled at 40 mg / L to 160 mg / L.

[0022] 14. A copper corrosion protection method, characterized in that the metal corrosion inhibition component described in 9 is adsorbed on the copper surface, and the fluorescence of the copper surface under ultraviolet light is used to perform corrosion inhibition treatment on the areas of the copper surface that have no fluorescence or have weaker fluorescence than other areas.

[0023] The present invention has the following beneficial technical effects:

[0024] 1. The present invention provides a method for preparing a metal corrosion inhibition component. The metal corrosion inhibition component has a large tetraphenylethylene group, but is easily adsorbed on the metal surface, and thus has excellent performance in protecting metals from hydrogen evolution corrosion.

[0025] 2. In the metal corrosion inhibition method of the present invention, it is easy to detect the concentration of the metal corrosion inhibition component in the corrosive medium. By detecting the concentration, targeted replenishment measures can be taken, thereby enabling convenient and timely corrosion protection.

[0026] Third, the metal corrosion inhibition components of the present invention can still emit strong visible fluorescence even when adsorbed and accumulated on metal surfaces. The copper corrosion protection method of the present invention utilizes the fluorescence effect of the metal corrosion inhibition components adsorbed on the copper surface to promptly detect potential corrosion hazards and achieve visual detection, thereby providing targeted and targeted corrosion protection and effectively preventing or reducing the occurrence of corrosion.

[0027] Other features and advantages of the present invention will be described in detail in the detailed description section. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 This is the hydrogen nuclear magnetic resonance spectrum of the product in Example 1.

[0029] Figure 2 This is the mass spectrum of the product of Example 1.

[0030] Figure 3 This is the hydrogen nuclear magnetic resonance spectrum of the product in Example 2.

[0031] Figure 4 This is the mass spectrum of the product of Example 2.

[0032] Figure 5 This is the UV-visible absorption spectrum of the product in Example 2.

[0033] Figure 6 This is a photo of the brass specimen under ultraviolet light after the corrosion test. DETAILED DESCRIPTION

[0034] The present invention is described in detail below in conjunction with specific embodiments. However, it should be noted that the protection scope of the present invention is not limited by these specific embodiments and principle explanations, but is determined by the claims.

[0035] In the present invention, except for the contents explicitly described, any matters or issues not mentioned are directly applicable to those known in the art without any changes. Moreover, any embodiment described herein can be freely combined with one or more other embodiments described herein, and the technical solutions or technical concepts formed thereby are considered part of the original disclosure or description of the present invention and should not be regarded as new content not disclosed or anticipated herein, unless a person skilled in the art considers that the combination is obviously unreasonable.

[0036] All features disclosed in this invention may be combined in any combination, and such combinations should be understood as disclosed or described in this invention. Unless a person skilled in the art considers such combination to be obviously unreasonable, such combinations should be considered as specifically disclosed and described in this invention. The numerical values ​​disclosed in this specification include not only the numerical values ​​specifically disclosed in the examples, but also the endpoints of the numerical ranges in this specification. The ranges of any combination of these numerical values ​​should be considered as the ranges disclosed or described in this invention.

[0037] Technical and scientific terms in the present invention shall be understood according to their definitions if they are defined, and shall be understood according to their general meanings in the art if they are not defined.

[0038] In the present invention, aminoethanol refers to NH2CH2CH2OH.

[0039] In the present invention, amino polyethylene glycol refers to NH2(CH2CH2O) m H,m>1.

[0040] In the present invention, the corrosive medium refers to an acidic medium containing water or consisting essentially of water.

[0041] In the present invention, the substituents on the benzene rings in the tetraphenylethylene derivative refer to the substituents on the four benzene rings of the tetraphenylethylene except for the vinyl group.

[0042] The present invention provides a method for preparing a metal corrosion inhibition component, comprising: reacting a compound represented by formula I with a compound represented by formula II in the presence of copper powder in a solvent-free or organic solvent;

[0043]

[0044]

[0045] wherein R1′, R2′ and R3′ are each independently a hydrogen atom, a hydrocarbon group or the same as X, X is —Cl, —Br or —I; and n is 0 to 50.

[0046] According to the preparation method of the present invention, the reaction is shown in the following chemical reaction formula:

[0047]

[0048] According to the preparation method of the present invention, the compound represented by Formula I only needs to meet the above definitions, and there are no other restrictions on R1', R2', and R3'. The compounds represented by Formula I and Formula II can be obtained commercially or produced by any known method. Based on the teachings of the present invention, those skilled in the art can select suitable raw materials to produce the metal corrosion inhibition component of the present invention based on cost and practical needs.

[0049] According to the preparation method of the present invention, in the compound represented by formula II, n is 0-30, preferably 0-16, and more preferably 0-12.

[0050] According to the preparation method of the present invention, in the compound represented by Formula I, one of R1', R2', and R3' is the same as X, and the remaining substituents are each independently a hydrogen atom or a hydrocarbon group; or two of R1', R2', and R3' are the same as X, and the other substituent is a hydrogen atom or a hydrocarbon group; or R1', R2', and R3' are all the same as X. The hydrocarbon group may be an alkyl group, a chain alkyl group such as a methyl group, an ethyl group, or a propyl group, or a cycloalkyl group, and the hydrocarbon group may also be an aryl group such as a phenyl group.

[0051] According to the preparation method of the present invention, in the compound represented by formula I, the substituents on the benzene ring (marked as ①, ②, ③, ④) can be located at any position on the benzene ring, that is, at the ortho, meta or para position of the vinyl group; preferably, the substituent on the benzene ring ④ is located at the para position of the vinyl group; more preferably, all substituents on the benzene ring are located at the para position of the vinyl group.

[0052] According to the preparation method of the present invention, the molar ratio of the compound of formula I, copper and the compound of formula II is 1:(0.01-1):(1-100), preferably 1:(0.03-0.5):(3-30).

[0053] In some embodiments, the compound of Formula I is 4-chlorotetraphenylethylene, 4-bromotetraphenylethylene, 4-iodotetraphenylethylene, di-(4-bromo)-tetraphenylethylene (cis or trans), or tetrakis-(4-bromo)-tetraphenylethylene.

[0054] According to the preparation method of the present invention, the compound of formula II is aminopolyethylene glycol or aminoethanol, wherein the hydrogen on the nitrogen atom will not react substantially if further substituted.

[0055] In some embodiments, the compound of formula II is aminoethanol, aminotriethylene glycol, aminotetraethylene glycol, or aminohexaethylene glycol.

[0056] According to the preparation method of the present invention, the reaction temperature is 80°C to 200°C.

[0057] According to the preparation method of the present invention, the reaction time is 2 hours to 168 hours.

[0058] According to the preparation method of the present invention, the reaction solvent is 1,4-dioxane, N,N'-dimethylformamide, N,N'-dimethylacetamide, dimethyl sulfoxide or N-methylpyrrolidone.

[0059] According to the preparation method of the present invention, after the reaction is completed, the clear liquid is separated and the solvent is removed to obtain the reaction product; alternatively, after the reaction is completed, water and an organic solvent are added for extraction, the organic phase is collected, and the organic solvent is removed to obtain the reaction product. Separation can be performed by centrifugation or filtration; the organic solvent used for extraction can be dichloromethane, chloroform, carbon tetrachloride, ether, or ethyl acetate; the organic solvent can be removed by any appropriate means, such as rotary evaporation; before removing the organic solvent, the organic phase can be dried, such as with a desiccant; the desiccant can be anhydrous sodium sulfate or anhydrous magnesium sulfate. The aforementioned reaction product can be further purified by column chromatography to obtain a purified reaction product.

[0060] The present invention also provides a metal corrosion inhibition component, which is prepared by the above method. The metal corrosion inhibition component can be a reaction product directly obtained after removing the organic solvent, or a reaction product after further purification.

[0061] The present invention also provides application of the metal corrosion inhibition component in protecting metal from hydrogen evolution corrosion.

[0062] According to the application of the present invention, the aforementioned metal corrosion inhibition component is suitable for an environment where hydrogen evolution corrosion exists, and is particularly suitable for an environment where hydrogen evolution corrosion mainly occurs or exists only.

[0063] According to the application of the present invention, the aforementioned metal corrosion inhibition component can be used in a strongly acidic environment. The strongly acidic environment can be an aqueous phase containing different concentrations of strong acids, such as one or more aqueous phases containing sulfuric acid, hydrochloric acid, mud acid, and aminosulfonic acid. The strongly acidic environment can be a pH < 3.

[0064] According to the application of the present invention, the aforementioned metal corrosion inhibition component can also be used in a weakly acidic environment. The weakly acidic environment can be an aqueous phase containing weak acids of varying concentrations, such as one or more aqueous phases containing formic acid, acetic acid, and citric acid, or one or more aqueous phases containing dissolved CO2, H2S, SO2, etc. The weakly acidic environment can have a pH value of 3 to 7.

[0065] The present invention also provides a metal corrosion inhibitor, which includes the above-mentioned metal corrosion inhibition component.

[0066] The present invention also provides a metal corrosion inhibition method, wherein the corrosive medium contains the aforementioned metal corrosion inhibition component. The concentration of the aforementioned metal corrosion inhibition component in the corrosive medium can be controlled within a range of 40 mg / L to 160 mg / L, preferably 60 mg / L to 140 mg / L, and more preferably 70 mg / L to 120 mg / L.

[0067] The present invention also provides another metal corrosion inhibition method, wherein the corrosive medium contains the aforementioned metal corrosion inhibition component, and the concentration of the metal corrosion inhibition component in the corrosive medium is detected and controlled by ultraviolet-visible absorption spectroscopy; preferably, the concentration of the metal corrosion inhibition component in the corrosive medium is controlled at 40 mg / L to 160 mg / L.

[0068] The present invention also provides a copper corrosion protection method, wherein the copper surface is adsorbed with the aforementioned metal corrosion inhibition component, and the fluorescence of the copper surface under ultraviolet light is used to perform corrosion inhibition treatment on areas of the copper surface that have no fluorescence or have weaker fluorescence than other areas.

[0069] According to the copper corrosion protection method of the present invention, the corrosion inhibition treatment is to supplement the adsorption of the aforementioned metal corrosion inhibition components.

[0070] The copper corrosion protection method of the present invention allows for targeted corrosion protection by simply adding corrosion inhibitor and repairing the protective film in areas where no corrosion inhibitor has been absorbed, no protective film has formed, or where the corrosion inhibitor has desorbed and the protective film is incomplete. This method saves reagents while providing efficient protection, thus achieving targeted corrosion protection. This can be easily implemented on flat metal surfaces, and even on the inner walls of metal pipes, with the aid of an endoscopic UV light source and dosing equipment, detection and targeted dosing can be achieved.

[0071] The present invention will be described in detail below with reference to specific examples. The following examples will help those skilled in the art to further understand the present invention, but are not intended to limit the present invention in any form.

[0072] Instruments and Tests

[0073] In the examples, nuclear magnetic resonance analysis (1H NMR) was performed using a Bruker Avance 400 MHz nuclear magnetic resonance spectrometer; mass spectrometry (TOF-MS) was performed using a Bruker Autoflex III-MALDI-TOF-MS time-of-flight mass spectrometer; and UV-visible absorption spectroscopy was performed using a Perkin Elmer Lambda 750 UV spectrophotometer.

[0074] Example 1

[0075] This example is used to illustrate the preparation method of the present invention.

[0076] The preparation method is shown in the following chemical reaction formula.

[0077]

[0078] The specific steps are as follows: 1.234 g of 4-bromotetraphenylethylene (3 mmol), 2 mg of copper powder (0.03 mmol), 0.184 g of aminoethanol (3 mmol), and 3 mL of 1,4-dioxane are added to a test tube. The mixture is heated to 80°C with magnetic stirring and reacted for 2 hours. The mixture is cooled to room temperature, and appropriate amounts of dichloromethane and water are added for separation and extraction. This process is repeated three times. The organic phase is collected, dried, filtered, and spin-dried. The mixture is then purified by column chromatography to obtain 0.413 g of the desired product as a yellow, viscous liquid.

[0079] 1H NMR (400MHz, DMSO): δ7.15-6.83 (15H, m), 6.65-6.55 (2H, d), 6.34-6.24 (2H, d), 3.56-3.50 (2H, t), 3.18-3.12 (2H, t).

[0080] MS (TOF-MS): [M+H + ]392.253.

[0081] Example 2

[0082] This example is used to illustrate the preparation method of the present invention.

[0083] The preparation method is shown in the following chemical reaction formula.

[0084]

[0085] The specific steps are as follows: 1.234 g of 4-bromotetraphenylethylene (3 mmol), 19.2 mg of copper powder (0.3 mmol), and 4.476 g of aminotriethylene glycol (30 mmol) are added to a test tube. The mixture is heated to 100°C with magnetic stirring and reacted for 24 hours. The mixture is cooled to room temperature, and appropriate amounts of dichloromethane and water are added for separation and extraction. This process is repeated three times. The organic phase is collected, dried, filtered, and spin-dried. The mixture is then purified by column chromatography to obtain 1.074 g of the desired product as a yellow, viscous liquid.

[0086] 1H NMR (400MHz, DMSO): δ7.20-6.85 (15H, m), 6.70-6.60 (2H, d), 6.40-6.30 (2H, d), 3.55-3.37 (10H, m), 3.15-3.05 (2H, m)

[0087] MS (TOF-MS): [M+H+ ]480.311.

[0088] Example 3

[0089] This example is used to illustrate the preparation method of the present invention.

[0090] The preparation method is shown in the following chemical reaction formula.

[0091]

[0092] The specific steps are as follows: 1.234 g of 4-bromotetraphenylethylene (3 mmol), 96 mg of copper powder (1.5 mmol), and 8.441 g of aminohexaethylene glycol (30 mmol) are added to a test tube. The mixture is heated to 140°C with magnetic stirring and reacted for 72 hours. The mixture is cooled to room temperature, and appropriate amounts of dichloromethane and water are added for separation and extraction. This process is repeated three times. The organic phase is collected, dried, filtered, and spin-dried. The mixture is then purified by column chromatography to obtain 1.139 g of the desired product as a yellow, viscous liquid.

[0093] Example 4

[0094] This example is used to illustrate the preparation method of the present invention.

[0095] The preparation method is shown in the following chemical reaction formula.

[0096]

[0097] The specific steps are as follows: 1.471 g of di-(4-bromo)tetraphenylethylene (3 mmol), 128 mg of copper powder (2 mmol), and 5.798 g of aminotetraethylene glycol (30 mmol) are added to a test tube. The mixture is heated to 160°C with magnetic stirring and reacted for 72 hours. The mixture is cooled to room temperature, and appropriate amounts of dichloromethane and water are added for separation and extraction. This process is repeated three times. The organic phase is collected, dried, filtered, and spin-dried. Purification by column chromatography yields 1.415 g of the desired product as a yellow, viscous liquid.

[0098] Example 5

[0099] This example is used to illustrate the preparation method of the present invention.

[0100] The preparation method is shown in the following chemical reaction formula.

[0101]

[0102] The specific steps are as follows: 1.944 g of tetrakis-(4-bromo)tetraphenylethylene (3 mmol), 192 mg of copper powder (3 mmol), and 57.98 g of aminotetraethylene glycol (300 mmol) are added to a test tube. The mixture is heated to 200°C with magnetic stirring and reacted for 168 hours. The mixture is cooled to room temperature, and appropriate amounts of dichloromethane and water are added. Separate extraction is repeated three times. The organic phase is collected, dried, filtered, and spin-dried. The mixture is then purified by column chromatography to obtain 1.817 g of the desired product as a yellow viscous liquid.

[0103] Example 6

[0104] Rotating coupon corrosion test

[0105] Prepare the corrosion solution: Dissolve 208g of concentrated H2SO4 in 4L of deionized water to make a 0.5M H2SO4 solution. Then, take 250mL of the 0.5M H2SO4 solution and place it in different glass bottles. Hang metal test pieces that have been treated with ethanol and weighed in these glass bottles in order, immersing the test pieces in the solution without touching the bottom or walls of the bottles. One bottle is left untreated as a blank test (i.e., Comparative Example 0). A certain concentration of the corrosion inhibition component products prepared in the above examples (i.e., Examples 1 to 5) and a certain concentration of the aminopolyethylene glycol and halogenated tetraphenylethylene raw materials in the above examples (i.e., Comparative Examples 1 to 3) are added. The glass bottles containing the corrosion solution and test pieces are placed in a rotary hanging instrument. The rotary hanging instrument is set to a temperature of 60°C, a rotation speed of 28 r / min, and a linear speed of 1 m / s. After a certain period of time, the test pieces are removed and treated with water, ethanol, etc., and then weighed. The mass loss of the test pieces before and after the test is calculated to obtain the corrosion inhibition performance of the agent.

[0106] The corrosion inhibition rate calculation formula is as follows:

[0107] η=(Δm0-Δm1) / Δm0×100

[0108] Where: η——corrosion inhibition rate, %

[0109] Δm0——mass loss of the test piece in the blank test, g

[0110] Δm1——mass loss of the test piece during the dosing test, g

[0111] Rotating coupon corrosion tests were conducted using the same method on H62 brass and N80 carbon steel specimens, with the exception of the test durations of 72 hours for brass and 4 hours for carbon steel. The results for the brass specimens are shown in Table 1, and the results for the carbon steel specimens are shown in Table 2.

[0112] The results in Table 1 show that for brass, the corrosion inhibition rate of the corrosion-inhibiting component of the present invention gradually increases with increasing agent concentration. When the agent concentration is 100 mg / L, the corrosion inhibition rates of Examples 1 to 5 all exceed 75%, with Examples 4 and 5 achieving inhibition rates exceeding 99%, demonstrating excellent corrosion inhibition performance. However, the aminopolyethylene glycol and halogenated tetraphenylethylene raw materials, i.e., Comparative Examples 1 to 3, exhibit poor corrosion inhibition performance, with inhibition rates below 25% at 100 mg / L.

[0113] The results in Table 2 show that for carbon steel, the corrosion inhibition rate of the corrosion-inhibiting component of the present invention gradually increases with increasing agent concentration. When the agent concentration is 100 mg / L, the corrosion inhibition rates of Examples 1 to 5 all exceed 70%, and the corrosion inhibition rates of Examples 2 to 5 exceed 95%, indicating excellent corrosion inhibition performance. However, the aminopolyethylene glycol and halogenated tetraphenylethylene raw materials, i.e., Comparative Examples 1 to 3, have poor corrosion inhibition performance, with corrosion inhibition rates below 25% at 100 mg / L.

[0114] Table 1

[0115] Drug concentration 40mg / L 70mg / L 100mg / L Comparative Example 0 - - - Example 1 40.6％ 57.7％ 75.3％ Example 2 59.9％ 77.3％ 83.7％ Example 3 74.9％ 86.9％ 93.9％ Example 4 91.1％ 94.9％ 99.0％ Example 5 94.9％ 96.9％ 99.3％ Comparative Example 1: Aminoethanol 14.3％ 17.1％ 18.8％ Comparative Example 2: Aminotriethylene glycol 16.0％ 19.2％ 21.2％ Comparative Example 3: Di-(4-bromo)-tetraphenylethylene -5.6％ 7.2％ 1.5％

[0116] Table 2

[0117] Drug concentration 40mg / L 70mg / L 100mg / L Comparative Example 0 - - - Example 1 40.1％ 55.6％ 72.8％ Example 2 52.5％ 88.3％ 95.9％ Example 3 73.3％ 89.2％ 96.3％ Example 4 90.1％ 92.6％ 96.8％ Example 5 91.7％ 95.1％ 97.6％ Comparative Example 1: Aminoethanol 10.8％ 13.9％ 17.7％ Comparative Example 2: Aminotriethylene glycol 12.3％ 21.7％ 24.7％ Comparative Example 3: Di-(4-bromo)-tetraphenylethylene -8.7％ -5.0％ 7.2％

[0118] Example 7

[0119] This example is used to illustrate the concentration determination of the compound of the present invention in a corrosive medium. Taking the product of Example 2 as an example, it was prepared into solutions of different mass concentrations using 0.5M H2SO4 as a solvent and subjected to UV-visible absorption spectrum measurement. Figure 5 As can be seen, the compound has a distinct UV absorption peak. A linear fit of the absorbance at 300nm, Abs, and the mass concentration, c, yields the relationship Abs = 0.02283c - 0.01067. When the corrosive medium contains an unknown concentration of the compound, the UV-Vis absorption spectrum of the solution can be measured to obtain the absorbance at 300nm. Substituting this into the above relationship yields the mass concentration of the compound in the corrosive medium. If the concentration is too high and the absorbance exceeds the measuring range, the sample should be diluted appropriately before measurement.

[0120] Example 8

[0121] This example is used to illustrate the fluorescence of the metal corrosion inhibition component of the present invention adsorbed on the copper surface.

[0122] After the corrosion test of the brass test piece in Example 6 was completed, the corrosion inhibition component product was adsorbed on the surface of the test pieces of Examples 1 to 5, and the test pieces showed a certain intensity of fluorescence under 365nm ultraviolet light; the test piece without adding any agent (Comparative Example 0) had no fluorescence under 365nm ultraviolet light; the test pieces containing amino polyethylene glycol and halogenated tetraphenylethylene raw materials with almost no corrosion inhibition performance (Comparative Examples 1 to Comparative Examples 3) had no fluorescence under 365nm ultraviolet light. Figure 6 From left to right, the photographs of the test pieces of Comparative Example 0, 100 mg / L Comparative Example 1, 100 mg / L Comparative Example 2, 100 mg / L Comparative Example 3, 100 mg / L Example 1, 100 mg / L Example 2, 100 mg / L Example 3, 100 mg / L Example 4, and 100 mg / L Example 5 after the corrosion test under 365 nm ultraviolet light are shown. It can be seen that the corrosion inhibition component of the present invention has a visual detection effect.

Claims

1. A method for preparing a metal corrosion inhibition component, comprising: In the absence of solvent or in an organic solvent, in the presence of copper powder, reacting the compound represented by formula I with the compound represented by formula II; wherein R1′, R2′ and R3′ are each independently a hydrogen atom, a hydrocarbon group or the same as X, X is —Cl, —Br or —I; and n is 0 to 50.

2. The preparation method according to claim 1, characterized in that: In the compound represented by formula II, n is 0-30.

3. The preparation method according to claim 2, characterized in that: In the compound represented by formula II, n is 0-16.

4. The preparation method according to claim 3, characterized in that: In the compound represented by formula II, n is 0-12.

5. The preparation method according to claim 1, characterized in that: One of R1', R2' and R3' is the same as X, and the remaining substituents are each independently a hydrogen atom or a hydrocarbon group; or two of R1', R2' and R3' are the same as X, and the other substituent is a hydrogen atom or a hydrocarbon group; or all of R1', R2' and R3' are the same as X.

6. The preparation method according to claim 1, characterized in that: The molar ratio of the compound of formula I, copper and the compound of formula II is 1:(0.01-1):(1-100).

7. The preparation method according to claim 6, characterized in that: The molar ratio of the compound of formula I, copper and the compound of formula II is 1:(0.03-0.5):(3-30).

8. The preparation method according to claim 1, characterized in that: The reaction temperature is 80°C to 200°C.

9. The preparation method according to claim 1, characterized in that: The reaction time is 2h~168h.

10. The preparation method according to claim 1, characterized in that: The reaction solvent is 1,4-dioxane, N,N'-dimethylformamide, N,N'-dimethylacetamide, dimethyl sulfoxide or N-methylpyrrolidone.

11. A metal corrosion inhibition component, characterized in that: Prepared by the method according to any one of claims 1 to 10.

12. Use of the metal corrosion inhibition component according to claim 11 in metal hydrogen evolution corrosion protection.

13. A metal corrosion inhibitor, characterized in that: The invention comprises the metal corrosion inhibition component according to claim 11.

14. A metal corrosion inhibition method, characterized in that: The corrosive medium contains the metal corrosion inhibition component according to claim 11.

15. A metal corrosion inhibition method, characterized in that: The corrosive medium contains the metal corrosion inhibition component according to claim 11, and the concentration of the metal corrosion inhibition component in the corrosive medium is detected and controlled by ultraviolet-visible absorption spectroscopy.

16. A method for protecting copper from corrosion, characterized in that: The copper surface is adsorbed with the metal corrosion inhibition component according to claim 11, and the fluorescence of the copper surface under ultraviolet light is used to perform corrosion inhibition treatment on areas of the copper surface that have no fluorescence or have weaker fluorescence than other areas.

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