CN112760658B - Corrosion inhibitor for dynamic cleaning of high Wen Xiaosuan washing liquid and preparation method thereof - Google Patents
Corrosion inhibitor for dynamic cleaning of high Wen Xiaosuan washing liquid and preparation method thereof Download PDFInfo
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- CN112760658B CN112760658B CN202110032002.9A CN202110032002A CN112760658B CN 112760658 B CN112760658 B CN 112760658B CN 202110032002 A CN202110032002 A CN 202110032002A CN 112760658 B CN112760658 B CN 112760658B
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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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/04—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors
- C23G1/06—Cleaning or pickling metallic material with solutions or molten salts with acid solutions using inhibitors organic inhibitors
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Abstract
The preparation method of the corrosion inhibitor for dynamic cleaning of the high Wen Xiaosuan washing liquid comprises the following raw materials in parts by mass: 2-4 parts of E-51 epoxy resin; 0.5-1 part of triglycidyl isocyanurate; 0.2-0.5 part of pentaerythritol tetraglycidyl ether; DMF 0.3-0.6 parts; 0.5-1 part of water; 0.08-0.15 part of 2-methylimidazole; 0.1-0.3 part of ethylenediamine; 0.5-0.8 part of ethanolamine. The corrosion inhibitor for dynamic cleaning of the high Wen Xiaosuan washing liquor has the advantages that the epoxy equivalent is more than 1500g/mol, the molecular weight is larger, the corrosion inhibitor cannot be damaged due to oxidization of nitric acid, and the corrosion inhibitor contains regular hydroxyl, amino, imidazoline ring and other groups, has strong and stable adsorption effect on metal base materials, has good water solubility and storage stability, and has excellent corrosion inhibition performance in the high-temperature dynamic cleaning process of the nitric acid washing liquor.
Description
Technical Field
The invention relates to the field of metal electroplating, in particular to a corrosion inhibitor for dynamic cleaning of high Wen Xiaosuan washing liquid used before metal electroplating and a preparation method thereof.
Background
Before the metal is electroplated or coated, an oxide film on the surface is generally removed through an acid washing step, so that the effects of excellent film adhesion and comprehensive performance of the subsequent coating are achieved.
For metals with fewer oxide films, ordinary normal-temperature acid washing is generally adopted, and hydrochloric acid solution is generally adopted for normal-temperature acid washing, so that on one hand, a small amount of chloride ions remain on the surface of the metal after acid washing to cause corrosion to follow-up processes.
For metal substrates with serious rust, high-temperature pickling is generally adopted to thoroughly clean the metal substrates, accelerate the oxide film removal speed and improve the production efficiency. The high temperature is typically around 80 ℃, the most commonly used pickling solution being nitric acid medium.
In the pickling step, in order to reduce the corrosion of the pickling solution to the metal substrate, and achieve the effect of removing the oxide film as much as possible and reducing the consumption of the metal substrate, a pickling corrosion inhibitor is generally added to the pickling solution. The acid pickling corrosion inhibitor has the binding capacity with the metal substrate, and an adsorption layer is formed on the surface of the metal substrate to achieve the function of isolating or slowing down the corrosion of the acid liquor on the metal substrate.
For the normal temperature pickling link, the corrosion inhibitor can be used in a large number of types, such as products with urotropine, thiourea, potassium thiocyanate, imidazoline and the like which are commonly used as main corrosion inhibitor components, and the corrosion inhibitor products have smaller molecules and are single molecular substances, so that a stable adsorption layer can be formed with the surface of the metal substrate at normal temperature.
However, in the high-temperature pickling process, the corrosion speed of the acid liquor is obviously enhanced due to high temperature, the molecular motion is aggravated, a single-molecule corrosion inhibitor cannot form a stable adsorption layer on the surface of a metal substrate, and desorption easily occurs to cause obvious reduction of corrosion inhibition capability. And for the nitric acid medium, the nitric acid medium has certain oxidizing capacity at high temperature, and single-molecule corrosion inhibitor products are oxidized to be deactivated, so that a large amount of metal base materials are lost in a medium-high temperature pickling link, and larger losses are brought to enterprises.
In order to solve the problem, related manufacturers have studied, for example, the products in ZL 2019102396. X are suitable for brass materials, the highest temperature can reach 50 ℃ of medium temperature, and the static corrosion inhibition effect is obvious. However, in order to improve the cleaning efficiency, manufacturers mostly adopt a high-temperature dynamic pickling method, and the corrosion inhibitor has a remarkably reduced corrosion inhibition effect under high-temperature dynamic conditions due to a small molecular weight.
Therefore, a new corrosion inhibitor suitable for dynamic cleaning of high Wen Xiaosuan washing liquid is needed to solve the technical problems.
Disclosure of Invention
In order to solve the technical problems, the invention provides a corrosion inhibitor for dynamic cleaning of high Wen Xiaosuan washing liquid and a preparation method thereof.
The invention relates to a preparation method of a corrosion inhibitor for dynamic cleaning of high Wen Xiaosuan lotion, which comprises the following raw materials in parts by mass:
the preparation method of the corrosion inhibitor for dynamic cleaning of the high-temperature nitric acid washing liquid further comprises the following steps:
A. stirring and mixing 2-methylimidazole, ethylenediamine and water in a formula amount at room temperature until the components are completely dissolved to obtain a mixed solution, and adding the mixed solution into a head tank for later use;
B. adding E-51 epoxy resin, triglycidyl isocyanurate, pentaerythritol tetraglycidyl ether and DMF (dimethyl formamide) in the formula amount into a reactor, and fully mixing at 35-40 ℃ until the mixture is dissolved into homogeneous phase;
C. uniformly dripping the mixed solution obtained in the step A into a reactor to react with the materials in the step B, and continuously carrying out heat preservation reaction for a period of time at 35-40 ℃ after dripping is finished;
D. when the epoxy equivalent of the system mixture is more than 500g/mol, adding the ethanolamine with the formula amount for chain extension reaction for a period of time;
D. stopping the reaction when the epoxy equivalent of the system mixture is more than 1500g/mol, and discharging to obtain the corrosion inhibitor for dynamic cleaning of the high-temperature nitric acid washing liquid.
Wherein in the step A, 2-methylimidazole, ethylenediamine and water are added into a mixer to be mixed.
In the step A, the mixed solution is pumped into a high-level tank for standby.
Wherein, the reactor is a reaction kettle.
Wherein, in the step C, the mixed solution obtained in the step A is dripped into the reactor by opening a control valve of an overhead tank filled with the mixed solution.
Wherein, in the step C, the dripping time is controlled to be 1.5-2.5h (preferably 2 h).
The invention also provides the corrosion inhibitor for dynamic cleaning of the high Wen Xiaosuan washing liquid, which is prepared by the preparation method of the corrosion inhibitor for dynamic cleaning of the high-temperature nitric acid washing liquid.
Wherein the corrosion inhibitor for dynamic cleaning of the high-temperature nitric acid washing liquid is a uniform viscous liquid in appearance, has a pH value of 8-9 and has an epoxy equivalent of more than 1500 g/mol.
Compared with the prior art, the invention has the following advantages:
1. the corrosion inhibitor for dynamic cleaning of the high-temperature nitric acid washing liquid is mainly prepared by using E-51 epoxy resin, triglycidyl isocyanurate, pentaerythritol tetraglycidyl ether, DMF, water, ethylenediamine, ethanolamine, 2-methylimidazole and the like as raw materials for reaction.
2. The corrosion inhibitor for dynamic cleaning of the high Wen Xiaosuan washing liquor has the advantages that the epoxy equivalent is more than 1500g/mol, the molecular weight is larger, the corrosion inhibitor cannot be damaged due to oxidization of nitric acid, and the corrosion inhibitor contains regular hydroxyl, amino, imidazoline ring and other groups, has strong and stable adsorption effect on metal base materials, has good water solubility and storage stability, and has excellent corrosion inhibition performance in the high-temperature dynamic cleaning process of the nitric acid washing liquor.
Detailed Description
The present invention will be further described in detail with reference to the following examples, which are given for the purpose of better understanding of the present invention, and therefore, are not to be construed as limiting the scope of the present invention, since numerous insubstantial modifications and adaptations of the invention will now occur to those skilled in the art in light of the teaching herein.
Example 1
The preparation method of the corrosion inhibitor for dynamic cleaning of the high Wen Xiaosuan washing liquid comprises the following raw materials in parts by mass:
further, the preparation method comprises the following steps:
A. adding 2-methylimidazole, ethylenediamine and water in the formula amount into a mixer, stirring and mixing at room temperature until the mixture is completely dissolved, and pumping the mixed solution into a high-level tank for later use;
B. adding E-51 epoxy resin, triglycidyl isocyanurate, pentaerythritol tetraglycidyl ether and DMF (dimethyl formamide) in the formula amount into a reaction kettle, and fully mixing at 35 ℃ until the mixture is dissolved into homogeneous phase;
C. c, opening a control valve of the overhead tank, uniformly dripping the mixed solution in the step A into the reaction kettle, controlling the dripping time to be 2.5h, and continuing to react at 35 ℃ for a period of time after finishing dripping;
D. when the epoxy equivalent of the system mixture is more than 500g/mol, adding the ethanolamine with the formula amount for chain extension reaction for a period of time;
D. stopping the reaction when the epoxy equivalent of the system mixture is more than 1500g/mol, and discharging to obtain the corrosion inhibitor for dynamic cleaning of the high-temperature nitric acid washing liquid.
Example 2
The preparation method of the corrosion inhibitor for dynamic cleaning of the high Wen Xiaosuan washing liquid comprises the following raw materials in parts by mass:
further, the preparation method comprises the following steps:
A. adding 2-methylimidazole, ethylenediamine and water in the formula amount into a mixer, stirring and mixing at room temperature until the mixture is completely dissolved, and pumping the mixed solution into a high-level tank for later use;
B. adding E-51 epoxy resin, triglycidyl isocyanurate, pentaerythritol tetraglycidyl ether and DMF (dimethyl formamide) in the formula amount into a reaction kettle, and fully mixing at 40 ℃ until the mixture is dissolved into homogeneous phase;
C. c, opening a control valve of the overhead tank, uniformly dripping the mixed solution in the step A into the reaction kettle, controlling the dripping time to be 1.5h, and continuing to react at 40 ℃ for a period of time after finishing dripping;
D. when the epoxy equivalent of the system mixture is more than 500g/mol, adding the ethanolamine with the formula amount for chain extension reaction for a period of time;
D. stopping the reaction when the epoxy equivalent of the system mixture is more than 1500g/mol, and discharging to obtain the corrosion inhibitor for dynamic cleaning of the high-temperature nitric acid washing liquid.
Example 3
The preparation method of the corrosion inhibitor for dynamic cleaning of the high Wen Xiaosuan washing liquid comprises the following raw materials in parts by mass:
further, the preparation method comprises the following steps:
A. adding 2-methylimidazole, ethylenediamine and water in the formula amount into a mixer, stirring and mixing at room temperature until the mixture is completely dissolved, and pumping the mixed solution into a high-level tank for later use;
B. adding E-51 epoxy resin, triglycidyl isocyanurate, pentaerythritol tetraglycidyl ether and DMF (dimethyl formamide) in the formula amount into a reaction kettle, and fully mixing at 37 ℃ until the mixture is dissolved into homogeneous phase;
C. c, opening a control valve of the overhead tank, uniformly dripping the mixed solution in the step A into the reaction kettle, controlling the dripping time to be 2.0h, and continuing to react at 37 ℃ for a period of time after finishing dripping;
D. when the epoxy equivalent of the system mixture is more than 500g/mol, adding the ethanolamine with the formula amount for chain extension reaction for a period of time;
D. stopping the reaction when the epoxy equivalent of the system mixture is more than 1500g/mol, and discharging to obtain the corrosion inhibitor for dynamic cleaning of the high-temperature nitric acid washing liquid.
Example 4
The preparation method of the corrosion inhibitor for dynamic cleaning of the high Wen Xiaosuan washing liquid comprises the following raw materials in parts by mass:
further, the preparation method comprises the following steps:
A. adding 2-methylimidazole, ethylenediamine and water in the formula amount into a mixer, stirring and mixing at room temperature until the mixture is completely dissolved, and pumping the mixed solution into a high-level tank for later use;
B. adding E-51 epoxy resin, triglycidyl isocyanurate, pentaerythritol tetraglycidyl ether and DMF (dimethyl formamide) in the formula amount into a reaction kettle, and fully mixing at 38 ℃ until the mixture is dissolved into homogeneous phase;
C. c, opening a control valve of the overhead tank, uniformly dripping the mixed solution in the step A into the reaction kettle, controlling the dripping time to be 1.8h, and continuing to react at 38 ℃ for a period of time after the dripping is finished;
D. when the epoxy equivalent of the system mixture is more than 500g/mol, adding the ethanolamine with the formula amount for chain extension reaction for a period of time;
D. stopping the reaction when the epoxy equivalent of the system mixture is more than 1500g/mol, and discharging to obtain the corrosion inhibitor for dynamic cleaning of the high-temperature nitric acid washing liquid.
Comparative example 1
Corrosion inhibition performance test was performed using the product of example 1 in ZL 20191021996. X as comparative example 1.
Comparative example 2
Corrosion inhibition performance test was performed using the product of example 1 in ZL201510879404.7 as comparative example 2.
Comparative example 3
Corrosion inhibition performance test was performed using the product of example 1 in ZL201810005486.6 as comparative example 3.
The test method of corrosion inhibition performance comprises the following steps:
the corrosion inhibition rate of the dynamic cleaning process is tested according to GB/T18175-2000 method for measuring corrosion inhibition performance of water treatment agent, wherein the washing liquid is tested by adopting a nitric acid solution with the mass concentration of 10% and a nitric acid solution with the mass concentration of 20%, and the addition mass of the corrosion inhibitor is 0.5% of the mass of the nitric acid washing liquid; time: 72h; washing liquid temperature: 80 ℃; test piece linear speed: 0.35m/s; test piece material: 20# carbon steel hanging piece.
The test results are shown in Table 1.
TABLE 1 results of Performance test of corrosion inhibitors prepared from examples and comparative examples
As can be seen from the comparison of examples 1-4 and comparative examples 1-3 in Table 1, the product of the invention has excellent corrosion inhibition performance in the dynamic cleaning process of nitric acid washing liquid at 80 ℃/72h through the mutual reaction and synergistic effect of the components, the dynamic corrosion inhibition rate is over 95% no matter the mass concentration is 10% or 20% of the nitric acid washing liquid, the product has excellent storage stability, and the phenomena of layering, sedimentation and the like do not occur in long-term storage.
The product in comparative example 1 is used as a corrosion inhibitor, after the amount of 0.5% of the mass of the nitric acid washing liquid is added, the weight loss is obvious after 80 ℃/72h of dynamic washing, the corrosion inhibition rate in the nitric acid washing liquid (the mass concentration is 10% or 20%) can only reach 87-91%, the corrosion inhibition rate is obviously lower than that of the product of the invention, and because the product is a compound product, a small amount of solid matters are settled after long-term storage.
The corrosion inhibitor products in comparative examples 2 and 3 have weak adsorption film layers due to small molecules and low solid content, and are easily damaged at high temperature and under dynamic cleaning, so that the corrosion inhibition effect is poor under the high temperature dynamic cleaning condition (80 ℃/72 h) for nitric acid washing liquid, and the corrosion inhibition performance is lower than 80%.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (7)
1. The preparation method of the corrosion inhibitor for dynamic cleaning of the high Wen Xiaosuan washing liquid comprises the following raw materials in parts by mass:
the preparation method comprises the following steps:
A. stirring and mixing 2-methylimidazole, ethylenediamine and water in a formula amount at room temperature until the components are completely dissolved to obtain a mixed solution, and adding the mixed solution into a head tank for later use;
B. adding E-51 epoxy resin, triglycidyl isocyanurate, pentaerythritol tetraglycidyl ether and DMF (dimethyl formamide) in the formula amount into a reactor, and fully mixing at 35-40 ℃ until the mixture is dissolved into homogeneous phase;
C. uniformly dripping the mixed solution obtained in the step A into a reactor to react with the materials in the step B, and continuously carrying out heat preservation reaction for a period of time at 35-40 ℃ after dripping is finished;
D. when the epoxy equivalent of the system mixture is more than 500g/mol, adding the ethanolamine with the formula amount for chain extension reaction for a period of time;
D. stopping the reaction when the epoxy equivalent of the system mixture is more than 1500g/mol, and discharging to obtain the corrosion inhibitor for dynamic cleaning of the high-temperature nitric acid washing liquid;
the corrosion inhibitor obtained has an epoxide equivalent of > 1500 g/mol.
2. The method for preparing a corrosion inhibitor according to claim 1, wherein in the step A, 2-methylimidazole, ethylenediamine and water are added into a mixer to be mixed.
3. The method for preparing corrosion inhibitor according to claim 1, wherein in the step A, the mixed solution is pumped into an elevated tank for standby.
4. The method for producing a corrosion inhibitor according to claim 1, wherein in the step C, the mixed solution obtained in the step A is dropped into the reactor by opening a control valve of an overhead tank containing the mixed solution.
5. The method for preparing a corrosion inhibitor according to claim 1, wherein in the step C, the dripping time is controlled to be 1.5-2.5 h.
6. The corrosion inhibitor for dynamic cleaning of high Wen Xiaosuan lotion, which is prepared by the method for preparing the corrosion inhibitor for dynamic cleaning of high Wen Xiaosuan lotion according to any one of claims 1 to 5.
7. The corrosion inhibitor for dynamic cleaning of high Wen Xiaosuan lotion according to claim 6, wherein the corrosion inhibitor has a pH of 8-9 and an epoxy equivalent of > 1500 g/mol.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102876185A (en) * | 2011-07-15 | 2013-01-16 | 日本帕卡濑精株式会社 | Drainage metal surface treating agent and metal material obtained by utilziing the same |
| US20140349015A1 (en) * | 2013-05-22 | 2014-11-27 | Jacam Chemical Company 2013, Llc | Corrosion inhibitor systems using environmentally friendly green solvents |
| CN109913879A (en) * | 2019-03-26 | 2019-06-21 | 大连理工大学 | A kind of Compositional type pyridine amidine corrosion inhibiter and preparation method thereof for nitric acid acidwashing brass part |
| CN110760863A (en) * | 2019-11-18 | 2020-02-07 | 黄山学院 | Corrosion inhibitor suitable for dynamic strong alkaline washing of metal workpiece and preparation method thereof |
-
2021
- 2021-01-11 CN CN202110032002.9A patent/CN112760658B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102876185A (en) * | 2011-07-15 | 2013-01-16 | 日本帕卡濑精株式会社 | Drainage metal surface treating agent and metal material obtained by utilziing the same |
| US20140349015A1 (en) * | 2013-05-22 | 2014-11-27 | Jacam Chemical Company 2013, Llc | Corrosion inhibitor systems using environmentally friendly green solvents |
| CN109913879A (en) * | 2019-03-26 | 2019-06-21 | 大连理工大学 | A kind of Compositional type pyridine amidine corrosion inhibiter and preparation method thereof for nitric acid acidwashing brass part |
| CN110760863A (en) * | 2019-11-18 | 2020-02-07 | 黄山学院 | Corrosion inhibitor suitable for dynamic strong alkaline washing of metal workpiece and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 环境友好型缓蚀剂的最新研究进展;韩跃飞等;《全面腐蚀控制》;20160528(第05期);第57-62页 * |
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