CN110129803B - Copper corrosion inhibitor based on metal organic framework materials MOFs and preparation method thereof - Google Patents
Copper corrosion inhibitor based on metal organic framework materials MOFs and preparation method thereof Download PDFInfo
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- CN110129803B CN110129803B CN201910293634.3A CN201910293634A CN110129803B CN 110129803 B CN110129803 B CN 110129803B CN 201910293634 A CN201910293634 A CN 201910293634A CN 110129803 B CN110129803 B CN 110129803B
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G83/008—Supramolecular polymers
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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
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Abstract
The invention belongs to the field of metal material corrosion inhibitors, and discloses a copper corrosion inhibitor based on metal organic framework materials MOFs (metal-organic frameworks) and a preparation method thereof, wherein the copper corrosion inhibitor comprises 20-40 parts by weight of aminobenzimidazole/Zn2+MOFs, 30-50 parts by weight of small molecular alcohol with molecular weight not more than 60 and 10-40 parts by weight of strong polar organic solvent with polarity not less than hexamethylphosphoramide, wherein the aminobenzimidazole/Zn2+MOFs have a structural formula shown in the following formula (I). The invention improves the key main material for forming the copper corrosion inhibitor, and adopts aminobenzimidazole/Zn2+MOFs as host materials, utilizing aminobenzimidazole/Zn2+The MOFs adsorption group has the characteristics of strong hydrophobicity and stable structure, and can play a good corrosion inhibition role on a copper simple substance or a copper alloy material.
Description
Technical Field
The invention belongs to the field of metal material corrosion inhibitors, and particularly relates to a copper corrosion inhibitor based on metal organic framework materials MOFs and a preparation method thereof.
Background
Copper is widely used as a structural material due to its excellent electrical and thermal conductivity, easy workability, and the like. However, copper is susceptible to corrosion during use, particularly in solutions containing chloride ions, which can cause structural failure. The corrosion inhibitor is added into a corrosion medium, which is the most convenient, efficient and economic means for inhibiting the corrosion of materials, and is widely applied in industry at present. But the copper corrosion inhibitor has fewer varieties and most of the corrosion inhibitors have lower corrosion inhibition performance; the corrosion inhibitor with good corrosion inhibition performance on copper, such as benzotriazole, has certain toxicity, so that a green and environment-friendly corrosion inhibitor with excellent corrosion inhibition performance is urgently needed in the market at present.
Metal-organic frameworks (MOFs)S) Is a novel crystalline porous material, and a regular porous network is formed by coordination of metal ion clusters, metal oxide clusters and an organic connecting agent. Because the MOFs have supramolecular properties, large specific surface area, abundant systems and heteroaryl topological structures, the MOFs have opened up an unprecedented opportunity for wide application since the 90 s of the 20 th century. MOFs are nontoxic because of their high boiling point and lack of volatility. In addition, the MOFs has stable structure and strong hydrophobicity, so that the requirements of the market on the copper corrosion inhibitor can be met by preparing the MOFs material with strong hydrophobicity and stable structure and having an adsorption group as the corrosion inhibitor.
Disclosure of Invention
In view of the above drawbacks or needs for improvement of the prior art, it is an object of the present invention to provide a copper corrosion inhibitor based on MOFs, a metal organic framework material, and a method for preparing the same, wherein the key host material constituting the copper corrosion inhibitor is modified by using aminobenzimidazole/Zn2+MOFs as host materials, utilizing aminobenzimidazole/Zn2+The MOFs adsorption group has the characteristics of strong hydrophobicity and stable structure, and can play a good corrosion inhibition role on a copper simple substance or a copper alloy material.
In order to achieve the above object, according to one aspect of the present invention, there is provided a copper corrosion inhibitor based on MOFs which is a metal organic framework material, characterized by comprising 20-40 parts by weight of aminobenzimidazole/Zn2+MOFs, 30-50 parts by weight of small molecular alcohol with molecular weight not more than 60 and 10-40 parts by weight of strong polar organic solvent with polarity not less than hexamethylphosphoramide, whereinThe amino benzimidazole/Zn2+MOFs have a structural formula as shown in formula (I):
according to another aspect of the present invention, the present invention provides a method for preparing the above copper corrosion inhibitor based on metal organic framework materials MOFs, which is characterized by comprising the following steps:
(1) taking a zincate and 2-aminobenzimidazole as raw materials, and reacting to generate MOFs (metal organic frameworks) shown in the following formula (I);
in addition, the molar ratio of zinc ions to 2-aminobenzimidazole in the raw materials meets 1: 2-2.6;
(2) and (2) stirring and mixing the MOFs obtained in the step (1) with small molecular alcohol and a strong polar organic solvent to obtain the copper corrosion inhibitor.
As a further preferred aspect of the present invention, in the step (1), the reaction is specifically a solvothermal reaction; preferably, the solvothermal reaction comprises two heating stages, and firstly, the reaction is carried out for 0.5 to 2 hours at the temperature of 60 to 90 ℃; then continuously heating, and carrying out heat preservation reaction at 120-160 ℃ for 18-36 hours;
the solvent used in the solvothermal reaction is an organic solvent, and before the reaction starts, the amount of the organic solvent is controlled to ensure that the concentration of zinc ions in a solution system is 0.2-0.3 mol/L.
As a further preferred aspect of the present invention, in the step (1), the zinc compound is at least one selected from the group consisting of zinc sulfate, zinc carbonate, zinc nitrate, and zinc nitrate tetrahydrate; the organic solvent is at least one selected from N-N dimethylformamide, formamide, dimethyl sulfoxide and N-N dimethylacetamide.
As a further preferred aspect of the present invention, in the step (2), the small molecule alcohol is at least one selected from methanol, ethanol, and isopropanol.
As a further preferred aspect of the present invention, in the step (2), the strongly polar organic solvent is at least one selected from the group consisting of N, N-dimethylformamide, formamide, and dimethyl sulfoxide.
According to another aspect of the present invention, the present invention provides an application of metal organic framework materials MOFs as host materials in copper corrosion inhibitors, which can effectively inhibit corrosion of copper simple substance or copper alloy material, wherein the metal organic framework materials MOFs are specifically aminobenzimidazole/Zn2+MOFs having a structural formula as shown in formula (I):
compared with the prior art, the technical scheme of the invention adopts aminobenzimidazole/Zn2+MOFs as key main material for forming copper corrosion inhibitor, amino benzimidazole/Zn is utilized2+The MOFs adsorption group has the characteristics of strong hydrophobicity and stable structure, and can play a good corrosion inhibition role on a copper simple substance or a copper alloy material.
The invention also relates to a method for preparing the amino benzimidazole/Zn by matching the small molecular alcohol with the molecular weight not more than 60 and the strong polar organic solvent with the polarity not less than hexamethylphosphoramide2+MOFs together form a copper corrosion inhibitor, wherein the small molecular alcohol has low viscosity, can be mutually dissolved with most solvents and can increase the content of aminobenzimidazole/Zn2+Fluidity of the MOFs solution; the strong polar organic solvent has good solubility, and can dissolve the synthesized MOFs solid, so that the corrosion inhibitor has good corrosion inhibition effect on the copper simple substance or the copper alloy material as a whole. In addition, the invention combines small molecular alcohol and strong polar organic solvent with aminobenzimidazole/Zn2+MOFs together form a copper corrosion inhibitor, and the aspects of non-toxicity, harmlessness, corrosion inhibition performance, economy and the like are comprehensively considered in the selection of reactants, the selection of small molecular alcohol and the selection of a strong polar organic solvent. Selecting aminobenzimidazole from various imidazoles and selecting zinc salt from various metal-containing salts; in the presence of a small molecule alcohol andin the selection of the strong polar solvent, the corresponding alcohol and the strong polar organic solvent are screened out through experiments in consideration of factors such as solubility, influence on reaction and the like. The invention is realized by mixing aminobenzimidazole/Zn2+The mass ratio of the MOFs, the small molecular alcohol and the strong polar organic solvent is controlled to be (20-40): (30-50): (10-40) the synthetic MOFs can be dissolved, and the corrosion inhibition effect is optimal.
Besides selecting aminobenzimidazole from various imidazoles and selecting zinc salt from various metal-containing salts, the invention also controls the proportion of a reactant zinc salt and aminobenzimidazole adopted by the synthesis process of the metal organic framework material MOFs, and controls the molar ratio of zinc ions and 2-aminobenzimidazole in the raw materials to be 1: 2-2.6, so as to obtain the metal organic framework material MOFs shown in the formula (I). The invention also preferably controls the amount of the solvent, the specific parameter conditions of the solvothermal reaction and the like in the synthesis of the metal organic framework material MOFs, successfully obtains the MOFs and further ensures the proper particle size of the MOFs. For central metal ions with flexible and diversified coordination modes and organic ligands with multiple coordination points, conditions are changed, and supermolecule isomerism is very easy to form, a zincate and 2-aminobenzimidazole are used as raw materials, organic solvents such as N-N dimethylformamide and the like are used as solvents to carry out solvothermal reaction, the solvothermal reaction is preferably controlled to be firstly carried out for 0.5-2 hours at the temperature of 60-90 ℃, then is carried out for 18-36 hours at the temperature of 120-160 ℃, and a metal organic framework material MOFs shown in a formula (I) can be generated; the heating is divided into two stages, the temperature and time of each stage are controlled, the MOFs can be synthesized smoothly, the two reactant raw materials can be fully reacted in the first stage at the temperature of 60-90 ℃ for 0.5-2 hours, the temperature is continuously increased to 120-160 ℃ in the second stage for 18-36 hours, a temperature condition can be provided for MOF growth, and therefore the whole process can provide a proper temperature condition for the reaction to facilitate the MOFs growth, and the finally obtained MOFs are suitable in particle size.
The copper corrosion inhibitor takes MOFs as a main component, and can effectively inhibit salt dissolutionCl in liquid-The corrosion inhibitor has small consumption (the consumption can be as low as 20ppm), obvious corrosion inhibition effect and environmental protection. In addition, the copper corrosion inhibitor can be used in different temperature environments (the temperature range can be 25-60 ℃, and the copper corrosion inhibitor has no volatility and toxicity), and can be directly added into a corrosion medium.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
In general, the corrosion inhibitor of the invention is prepared from 20-40 parts by weight of aminobenzimidazole/Zn2+MOFs, 30-50 parts by weight of micromolecular alcohol and 10-40 parts by weight of strong polar organic solvent.
The reaction in the preparation process of the corrosion inhibitor is as follows:
the following are specific examples:
example 1:
adding 56 g of zinc nitrate, 50 g of 2-aminobenzimidazole and 800mL of N, N-dimethylformamide into a beaker, stirring and dissolving, uniformly mixing, transferring into a closed hydrothermal kettle, carrying out heated solvothermal reaction, and keeping the temperature for reaction for 1 hour when the reaction temperature reaches 80 ℃; continuously heating to 140 ℃, maintaining the temperature and reacting for 24 hours to obtain aminobenzimidazole/Zn2+MOFs. 20 g of aminobenzimidazole/Zn prepared above were added to a beaker2+MOFs, 40 g of isopropanol, 40 g of N, N-dimethylformamide, 100 g of copper corrosion inhibitor was obtained.
Evaluating the corrosion inhibition performance:
the corrosion inhibition performance of the copper corrosion inhibitor on red copper is evaluated by adopting a weight loss hanging piece method at 25 ℃ and 0.5M NaCl solution, and the weight loss hanging piece time is 72 hours. Table 1 shows the results of comparative evaluation of the corrosion inhibitor of the present invention and commercially available methylbenzotriazole.
TABLE 1
As can be seen from the test data in Table 1, in an evaluation system, the corrosion inhibitor has a remarkable inhibition effect on corrosion of red copper, and simultaneously, the corrosion inhibition performance is superior to that of a commercial methylbenzotriazole product.
Example 2:
adding 28 g of zinc sulfate, 60 g of 2-aminobenzimidazole and 700mL of N, N-dimethylformamide into a beaker, stirring and dissolving, uniformly mixing, transferring into a closed hydrothermal kettle, carrying out heated solvothermal reaction, and keeping the temperature for reaction for 0.5 hour when the reaction temperature reaches 60 ℃; continuously heating to 120 ℃, maintaining the temperature and reacting for 18 hours to obtain aminobenzimidazole/Zn2+MOFs。
40 g of aminobenzimidazole/Zn prepared above were added to a beaker2+MOFs, 30 g methanol, 30 g formamide, 100 g copper corrosion inhibitor was obtained.
Evaluating the corrosion inhibition performance:
the corrosion inhibition performance of the copper corrosion inhibitor on red copper is evaluated by adopting a weight loss hanging piece method at 50 ℃ and 0.3M NaCl solution, and the weight loss hanging piece time is 72 hours. Table 2 shows the comparative evaluation results of the corrosion inhibitor of the present invention and the commercially available benzotriazole.
TABLE 2
As can be seen from the test data in Table 2, in an evaluation system, the corrosion inhibitor has a remarkable corrosion inhibition effect on red copper, and the corrosion inhibition performance is superior to that of a commercial benzotriazole product.
Example 3:
adding 60 g of zinc nitrate, 65 g of 2-aminobenzimidazole and 1000mL of N, N-dimethylformamide into a beaker, stirring and dissolving, uniformly mixing, transferring into a closed hydrothermal kettle, carrying out heated solvothermal reaction, and keeping the temperature for reaction for 2 hours when the reaction temperature reaches 90 ℃; continuously heating to 160 ℃, maintaining the temperature and reacting for 36 hours to obtain aminobenzimidazole/Zn2+MOFs。
30 g of aminobenzimidazole/Zn prepared above were added to a beaker2+MOFs, 40 g ethanol, 30 g formamide, 100 g copper corrosion inhibitor was obtained.
Evaluating the corrosion inhibition performance:
the corrosion inhibition performance of the copper corrosion inhibitor on red copper is evaluated by adopting a weight loss hanging piece method at 60 ℃ and 0.2M NaCl solution, and the weight loss hanging piece time is 72 hours. Table 3 shows the results of comparative evaluation of the corrosion inhibitors of the invention and commercially available mercaptobenzothiazoles.
TABLE 3
As can be seen from the test data in Table 3, in an evaluation system, the corrosion inhibitor has a remarkable corrosion inhibition effect on red copper, and simultaneously, the corrosion inhibition performance is superior to that of a commercial mercaptobenzothiazole product.
In addition to the N, N-dimethylformamide and N-dimethylacetamide used in the solvothermal reaction in the above examples, dimethyl sulfoxide, formamide, and the like can be used as a solvent as long as the reactants can be dissolved, have a high boiling point (not less than 120 ℃), and do not decompose and participate in the reaction at all heating stages of the solvothermal reaction.
Copper corrosion inhibitors of the invention, other than aminobenzimidazole/Zn2+Besides the MOFs, the small molecular alcohol and the strong polar organic solvent, other functional components can be added according to actual needs, such as a surfactant with solubilization and dispersion effects, a scale inhibitor with metal scale inhibition effect, a bactericide with sterilization effect and the like.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A copper corrosion inhibitor based on MOFs (metal organic frameworks) is characterized by comprising 20-40 parts by weight of aminobenzimidazole/Zn2+MOFs, 30-50 parts by weight of small molecular alcohol with molecular weight not more than 60 and 10-40 parts by weight of strong polar organic solvent with polarity not less than hexamethylphosphoramide, wherein the aminobenzimidazole/Zn2+MOFs have a structural formula as shown in formula (I):
and the strong polar organic solvent is at least one selected from N, N-dimethylformamide, formamide and dimethyl sulfoxide.
2. The method for preparing the copper corrosion inhibitor based on the MOFs (metal organic frameworks) of the claim 1, which is characterized by comprising the following steps:
(1) taking a zincate and 2-aminobenzimidazole as raw materials, and reacting to generate MOFs (metal organic frameworks) shown in the following formula (I);
in addition, the molar ratio of zinc ions to 2-aminobenzimidazole in the raw materials meets 1: 2-2.6;
(2) stirring and mixing the MOFs obtained in the step (1) with small molecular alcohol and a strong polar organic solvent to obtain a copper corrosion inhibitor; wherein the strong polar organic solvent is at least one selected from N, N-dimethylformamide, formamide and dimethyl sulfoxide.
3. The method according to claim 2, wherein in the step (1), the reaction is specifically a solvothermal reaction; the solvothermal reaction comprises two heating stages, and firstly, the reaction is carried out for 0.5 to 2 hours at the temperature of between 60 and 90 ℃ in a heat preservation manner; then continuously heating, and carrying out heat preservation reaction at 120-160 ℃ for 18-36 hours;
the solvent used in the solvothermal reaction is an organic solvent, and before the reaction starts, the amount of the organic solvent is controlled to ensure that the concentration of zinc ions in a solution system is 0.2-0.3 mol/L.
4. The method according to claim 3, wherein in the step (1), the zinc compound is at least one selected from the group consisting of zinc sulfate, zinc carbonate, zinc nitrate, and zinc nitrate tetrahydrate; the organic solvent is at least one selected from N-N dimethylformamide, formamide, dimethyl sulfoxide and N-N dimethylacetamide.
5. The method according to any one of claims 2 to 4, wherein in the step (2), the small molecule alcohol is at least one selected from methanol, ethanol and isopropanol.
6. The application of the MOFs as a main material in a copper corrosion inhibitor can effectively inhibit the corrosion of a copper simple substance or a copper alloy material, and is characterized in that the MOFs is specifically aminobenzimidazole/Zn2+MOFs having a structural formula as shown in formula (I):
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