CN111362883A - Benzotriazole derivative corrosion inhibitor and preparation method and application thereof - Google Patents
Benzotriazole derivative corrosion inhibitor and preparation method and application thereof Download PDFInfo
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- CN111362883A CN111362883A CN202010297846.1A CN202010297846A CN111362883A CN 111362883 A CN111362883 A CN 111362883A CN 202010297846 A CN202010297846 A CN 202010297846A CN 111362883 A CN111362883 A CN 111362883A
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- benzotriazole
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D249/00—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms
- C07D249/16—Heterocyclic compounds containing five-membered rings having three nitrogen atoms as the only ring hetero atoms condensed with carbocyclic rings or ring systems
- C07D249/18—Benzotriazoles
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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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Abstract
The invention relates to a benzotriazole derivative corrosion inhibitor and a preparation method and application thereof, wherein the preparation method comprises the following steps: placing benzotriazole, diethanolamine and formaldehyde into a reaction vessel for mixing to obtain a mixed raw material; heating the mixed raw materials to 85-110 ℃ while stirring, and then carrying out heat preservation reaction for a preset time; cooling to room temperature to obtain the product. The prepared copper corrosion inhibitor of the benzotriazole derivatives has excellent hydrophilicity, can be directly used without being converted into water-soluble salt and then used, has good corrosion-retarding performance, and is not limited by European Union REACH specifications; in addition, the preparation method of the benzotriazole derivative corrosion inhibitor is simple and is easy to apply to industrial production.
Description
Technical Field
The invention relates to the technical field of chemical reagents, in particular to a benzotriazole derivative corrosion inhibitor and a preparation method and application thereof.
Background
The corrosion of metal equipment and workpieces is always a serious problem faced by various production and processing enterprises at present, which not only causes serious capital loss, increase of production cost and reduction of production efficiency of the enterprises, but also causes certain resource waste. Copper has the characteristics of good processability, mechanical strength, thermal conductivity, electrical conductivity, corrosion resistance and the like, and is widely applied to various processing and manufacturing enterprises, the electronic industry and other fields. Large number of application fields and use numbersOne aspect that must be considered is the corrosion protection of copper. Although metallic copper has good corrosion resistance, it is used in special application environments, such as oxygen-containing water, acidic solutions, CN-containing solutions-Or NH4+Ionic aqueous solutions, etc., can cause severe corrosion to copper. Therefore, in order to effectively inhibit the occurrence of copper corrosion, a copper corrosion inhibitor is used in many ways at present. The copper corrosion inhibitor used in China mainly comprises thiourea, aldehyde, aniline, amine derivatives, thiazole and other organic heterocyclic compounds, such as benzotriazole with larger dosage. However, benzotriazole can not be used alone due to poor water solubility, and is required to be neutralized with organic amine or inorganic base, so that the convenience of benzotriazole is greatly reduced.
Disclosure of Invention
Therefore, it is necessary to provide a preparation method of a benzotriazole derivative corrosion inhibitor, aiming at the problems, the prepared benzotriazole derivative corrosion inhibitor has excellent hydrophilicity, can achieve the traditional equivalent copper corrosion inhibition effect, has a simple preparation method, and is easy to apply to industrial production.
A preparation method of a benzotriazole derivative corrosion inhibitor comprises the following steps:
placing benzotriazole, diethanolamine and formaldehyde into a reaction vessel for mixing to obtain a mixed raw material;
heating the mixed raw materials to 85-110 ℃ while stirring, and then carrying out heat preservation reaction for a preset time;
cooling to room temperature to obtain the product.
According to the preparation method of the benzotriazole derivative corrosion inhibitor, the prepared benzotriazole derivative copper corrosion inhibitor has excellent hydrophilicity, can be directly used without being converted into water-soluble salt and then used, has good corrosion inhibition performance, and is not limited by European Union REACH specifications; in addition, the preparation method of the benzotriazole derivative corrosion inhibitor is simple and is easy to apply to industrial production.
In one embodiment, the molar ratio of benzotriazole, diethanolamine and formaldehyde is 1-1.5: 1: 1 to 1.5.
In one embodiment, the molar ratio of benzotriazole, diethanolamine and formaldehyde is 1.4-1.5: 1: 1.2 to 1.5.
In one embodiment, the molar ratio of benzotriazole, diethanolamine and formaldehyde is 1.5: 1: 1.3 to 1.5.
In one embodiment, the formaldehyde is a 37wt% to 40 wt% formaldehyde solution.
In one embodiment, the reaction time is 3-10 hours.
The invention also provides a benzotriazole derivative corrosion inhibitor prepared by adopting the preparation method of the benzotriazole derivative corrosion inhibitor, which has excellent hydrophilicity, can be directly used without being converted into water-soluble salt and then used, and has good corrosion-inhibiting performance.
In one embodiment, the benzotriazole derivative has the structure:
in one embodiment, the mass content of the benzotriazole derivative in the benzotriazole derivative corrosion inhibitor is 85-95%.
The benzotriazole derivative corrosion inhibitor can be applied as a copper corrosion inhibitor, and has a good corrosion prevention effect.
Drawings
FIG. 1 is a graph comparing the results of the benzotriazole derivative corrosion inhibitor of example 5 with the results of the comparative examples.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The invention provides a preparation method of a benzotriazole derivative corrosion inhibitor, which comprises the following steps:
s100: and (2) placing benzotriazole, diethanolamine and formaldehyde into a reaction vessel for mixing to obtain a mixed raw material.
In one embodiment, the molar ratio of benzotriazole, diethanolamine and formaldehyde is 1-1.5: 1: 1 to 1.5. Preferably, the molar ratio of benzotriazole, diethanolamine and formaldehyde is 1.4-1.5: 1: 1.2-1.5, the yield of the benzotriazole derivatives is high, and the reaction efficiency is high. Optimally, the molar ratio of benzotriazole, diethanolamine and formaldehyde is 1.5: 1: 1.3-1.5, the yield of the benzotriazole derivatives is high, the reaction efficiency is high, the benzotriazole derivatives can be diluted with water to a larger concentration range in use, and the application is more flexible.
In one embodiment, the formaldehyde is a 37wt% to 40 wt% formaldehyde solution. Benzotriazole and diethanolamine
S200: heating the mixed raw materials to 85-110 ℃ while stirring, and then carrying out heat preservation reaction for a preset time. Preferably, the reaction time is 3-10 hours, so that the mixed raw materials can fully react. The reaction process adopts a mode of normal pressure reflux, so that the raw materials can react for a long time.
Benzotriazole, diethanolamine and formaldehyde are subjected to condensation reaction in the step, and the reaction equation is as follows:
the structure of the benzotriazole derivative is as follows:
s300: cooling to room temperature to obtain the product.
The invention also provides a benzotriazole derivative corrosion inhibitor prepared by the preparation method of the benzotriazole derivative corrosion inhibitor.
In one embodiment, the mass content of the benzotriazole derivative in the benzotriazole derivative corrosion inhibitor is 85-95%.
The benzotriazole derivative corrosion inhibitor can be applied as a copper corrosion inhibitor or corrosion inhibitors of other metals, and the corrosion inhibition effect of copper is optimal.
According to the preparation method of the benzotriazole derivative corrosion inhibitor, the prepared benzotriazole derivative copper corrosion inhibitor has excellent hydrophilicity, can be directly used without being converted into water-soluble salt and then used, and has good corrosion inhibition performance. Moreover, the preparation method of the benzotriazole derivative corrosion inhibitor can obtain a good condensation reaction result without adding other raw materials, the generation rate of the benzotriazole derivative serving as an active ingredient is high, the benzotriazole derivative can be directly taken for use after production is finished, the benzotriazole derivative is not required to be converted into water-soluble salt firstly, the generated product is not limited by European Union REACH specifications for use, the generation and treatment processes of impurities are reduced, the operation is simple, and the benzotriazole derivative corrosion inhibitor is easy to apply to industrial production.
The following are descriptions of specific embodiments.
Example 1
The preparation method of the benzotriazole derivative corrosion inhibitor of the embodiment comprises the following steps:
s100: mixing a mixture of 1: 1: 1, placing benzotriazole, diethanol amine and formaldehyde in a reaction vessel for mixing to obtain a mixed raw material.
The formaldehyde is 37-40 wt% formaldehyde solution.
S200: the temperature of the mixed raw materials is raised to 90 ℃ while stirring, and then the reaction is carried out for 4 hours under the condition of heat preservation.
S300: and cooling to room temperature to obtain the product benzotriazole derivative corrosion inhibitor, wherein the mass content of the benzotriazole derivative in the benzotriazole derivative corrosion inhibitor is 88%.
Example 2
The preparation method of the benzotriazole derivative corrosion inhibitor of the embodiment comprises the following steps:
s100: mixing the components in a molar ratio of 1.2: 1: 1.4, placing benzotriazole, diethanol amine and formaldehyde in a reaction vessel for mixing to obtain a mixed raw material.
The formaldehyde is 37-40 wt% formaldehyde solution.
S200: heating the mixed raw materials to 86 ℃ while stirring, and then carrying out heat preservation reaction for 8 hours.
S300: and cooling to room temperature to obtain the product benzotriazole derivative corrosion inhibitor, wherein the mass content of the benzotriazole derivative in the benzotriazole derivative corrosion inhibitor is 87%.
Example 3
The preparation method of the benzotriazole derivative corrosion inhibitor of the embodiment comprises the following steps:
s100: mixing the components in a molar ratio of 1.4: 1: 1.3, placing benzotriazole, diethanol amine and formaldehyde in a reaction vessel for mixing to obtain a mixed raw material.
The formaldehyde is 37-40 wt% formaldehyde solution.
S200: heating the mixed raw materials to 95 ℃ while stirring, and then carrying out heat preservation reaction for 10 hours.
S300: and cooling to room temperature to obtain the product benzotriazole derivative corrosion inhibitor, wherein the mass content of the benzotriazole derivative in the benzotriazole derivative corrosion inhibitor is 93%.
Example 4
The preparation method of the benzotriazole derivative corrosion inhibitor of the embodiment comprises the following steps:
s100: and (3) mixing the raw materials in a molar ratio of 1-1.5: 1: 1.4, placing benzotriazole, diethanol amine and formaldehyde in a reaction vessel for mixing to obtain a mixed raw material.
The formaldehyde is 37-40 wt% formaldehyde solution.
S200: the temperature of the mixed raw materials is raised to 105 ℃ while stirring, and then the reaction is carried out for 7 hours under the condition of heat preservation.
S300: and cooling to room temperature to obtain the product benzotriazole derivative corrosion inhibitor, wherein the mass content of the benzotriazole derivative in the benzotriazole derivative corrosion inhibitor is 94%.
Example 5
The preparation method of the benzotriazole derivative corrosion inhibitor of the embodiment comprises the following steps:
s100: mixing the components in a molar ratio of 1.5: 1: 1.5, placing benzotriazole, diethanol amine and formaldehyde in a reaction vessel for mixing to obtain a mixed raw material.
The formaldehyde is 37-40 wt% formaldehyde solution.
S200: heating the mixed raw materials to 85-110 ℃ while stirring, and then carrying out heat preservation reaction for 3-10 hours.
S300: and cooling to room temperature to obtain the product benzotriazole derivative corrosion inhibitor, wherein the mass content of the benzotriazole derivative in the benzotriazole derivative corrosion inhibitor is 91%.
Example 6
The preparation method of the benzotriazole derivative corrosion inhibitor of the embodiment comprises the following steps:
s100: mixing the components in a molar ratio of 1.5: 1: 1.3, placing benzotriazole, diethanol amine and formaldehyde in a reaction vessel for mixing to obtain a mixed raw material.
The formaldehyde is 37-40 wt% formaldehyde solution.
S200: heating the mixed raw materials to 110 ℃ while stirring, and then carrying out heat preservation reaction for 5 hours.
S300: and cooling to room temperature to obtain the product benzotriazole derivative corrosion inhibitor, wherein the mass content of the benzotriazole derivative in the benzotriazole derivative corrosion inhibitor is 90%.
Application test
The benzotriazole derivative corrosion inhibitors of examples 1 to 6 were compared with commercially available rust inhibitors T706.
Preparing a reagent: adding water into the benzotriazole derivative corrosion inhibitor of the example 1 to enable the mass fraction of the benzotriazole derivative corrosion inhibitor to be 0.1%, adding 100ppm of active sulfur, and adjusting the pH value to 9.5-10 by adopting monoethanolamine to obtain the experimental reagent of the example 1.
The test reagents of examples 2 to 6 and the test reagent of the commercial rust preventive T706 were prepared in the same manner.
The test reagents of examples 1 to 6 and the test reagent of the commercial rust inhibitor T706 were subjected to the copper corrosion test according to GB6144-2010, respectively, and compared with a blank sample, which did not undergo any corrosion protection on the copper sample, and the test results are shown in Table 1.
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | T706 | Blank sample | |
| Grade of corrosion resistance | 1a | 1a | 1a | 1a | 1a | 1a | 1b | 4b |
FIG. 1 shows the comparison between the test reagent of example 5 and the test reagent of a commercially available rust inhibitor T706, wherein A is the test reagent of example 5 and B is the test reagent of the commercially available rust inhibitor T706.
As can be seen from Table 1 and FIG. 1, the benzotriazole derivative corrosion inhibitor prepared by the invention has better corrosion resistance.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express one embodiment of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the benzotriazole derivative corrosion inhibitor is characterized by comprising the following steps:
placing benzotriazole, diethanolamine and formaldehyde into a reaction vessel for mixing to obtain a mixed raw material;
heating the mixed raw materials to 85-110 ℃ while stirring, and then carrying out heat preservation reaction for a preset time;
cooling to room temperature to obtain the product.
2. The preparation method of the benzotriazole derivative corrosion inhibitor according to claim 1, wherein the molar ratio of benzotriazole, diethanolamine and formaldehyde is 1-1.5: 1: 1 to 1.5.
3. The preparation method of the benzotriazole derivative corrosion inhibitor according to claim 2, wherein the molar ratio of benzotriazole, diethanolamine and formaldehyde is 1.4-1.5: 1: 1.2 to 1.5.
4. The preparation method of the benzotriazole derivative corrosion inhibitor according to claim 2, wherein the molar ratio of benzotriazole, diethanolamine and formaldehyde is 1.5: 1: 1.3 to 1.5.
5. The preparation method of the benzotriazole derivative corrosion inhibitor according to any one of claims 1 to 4, wherein the formaldehyde is a 37wt% to 40 wt% formaldehyde solution.
6. The preparation method of the benzotriazole derivative corrosion inhibitor according to claim 1, wherein the reaction time for heat preservation is 3-10 hours.
7. The benzotriazole derivative corrosion inhibitor prepared by the preparation method of the benzotriazole derivative corrosion inhibitor of any one of claims 1 to 6.
8. The benzotriazole derivative corrosion inhibitor of claim 7, wherein the benzotriazole derivative has the structure:
9. the benzotriazole derivative corrosion inhibitor of claim 7 or 8, wherein the mass content of the benzotriazole derivative in the benzotriazole derivative corrosion inhibitor is 85-95%.
10. Use of the benzotriazole derivative corrosion inhibitor of any one of claims 7-9 as a copper corrosion inhibitor.
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| PCT/CN2021/077714 WO2021208602A1 (en) | 2020-04-16 | 2021-02-24 | Benzotriazole derivative corrosion inhibitor, preparation method therefor and use thereof |
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Cited By (5)
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| CN112028845A (en) * | 2020-08-05 | 2020-12-04 | 长江大学 | Copper corrosion inhibitor and preparation method thereof |
| WO2021208602A1 (en) * | 2020-04-16 | 2021-10-21 | 安美科技股份有限公司 | Benzotriazole derivative corrosion inhibitor, preparation method therefor and use thereof |
| CN113620895A (en) * | 2021-09-09 | 2021-11-09 | 中国科学院兰州化学物理研究所 | Multifunctional lubricating additive and preparation method thereof |
| CN115850196A (en) * | 2022-11-29 | 2023-03-28 | 河北宝力工程装备股份有限公司 | Non-phosphorus multifunctional high-efficiency corrosion inhibitor and preparation method thereof |
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| CN113620895A (en) * | 2021-09-09 | 2021-11-09 | 中国科学院兰州化学物理研究所 | Multifunctional lubricating additive and preparation method thereof |
| CN115850196A (en) * | 2022-11-29 | 2023-03-28 | 河北宝力工程装备股份有限公司 | Non-phosphorus multifunctional high-efficiency corrosion inhibitor and preparation method thereof |
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Also Published As
| Publication number | Publication date |
|---|---|
| WO2021208602A1 (en) | 2021-10-21 |
| WO2021208602A9 (en) | 2021-11-18 |
| CN111362883B (en) | 2022-04-19 |
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