CN108070864B - pH value response intelligent control release corrosion inhibitor and preparation method thereof - Google Patents
pH value response intelligent control release corrosion inhibitor and preparation method thereof Download PDFInfo
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- CN108070864B CN108070864B CN201711425005.9A CN201711425005A CN108070864B CN 108070864 B CN108070864 B CN 108070864B CN 201711425005 A CN201711425005 A CN 201711425005A CN 108070864 B CN108070864 B CN 108070864B
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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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- 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
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Abstract
The invention belongs to the technical field of macromolecules and discloses a pH value response intelligent control release corrosion inhibition capsule and a preparation method thereof, wherein the pH value response intelligent control release corrosion inhibitor consists of a pH response capsule and a corrosion inhibition medicament; the pH response capsule wraps the corrosion inhibition agent, when the material is corroded, the pH of the environment rises, the capsule swells, and the corrosion inhibition agent is released; adding vinyltriethoxysilane and ethylene glycol monomethyl ether into a 250mL three-neck flask, and adding an initiator azodiisobutyronitrile and a corrosion inhibition medicament Benzotriazole (BTA); gradually dripping acrylic acid and octadecyl acrylate into the reaction solution through a constant pressure funnel, after finishing dripping within 2 hours, after reacting for 3 hours, adding N, N' -dimethylene bisacrylamide, continuing to react for 2 hours, adding Polyethyleneimine (PEI), stirring for 0.5 hour, taking out, and removing a solvent ethylene glycol monomethyl ether by vacuum drying. The invention prolongs the corrosion protection action time of the corrosion inhibitor.
Description
Technical Field
The invention belongs to the technical field of macromolecules, and particularly relates to a pH value response intelligent control release corrosion inhibition capsule and a preparation method thereof.
Background
The corrosion inhibitor is a single compound or a mixture of different compounds which exists in a corrosion medium in a proper concentration and a specific form and can prevent or slow down a metal reaction process, and can be divided into inorganic, organic, natural plant extracts and compound corrosion inhibitors according to the composition structure. The inorganic corrosion inhibitor is an oxide for promoting metal passivation or inorganic salts capable of forming a film on the metal surface, such as sodium nitrite, chromate, trisodium phosphate and the like; the organic corrosion inhibitor is an organic matter containing functional groups or unsaturated bonds of elements such as O, N, P, S and the like in a composition structure, and can form coordinate bonds with metal atoms to generate a film on the surface of a sample, so that the purpose of inhibiting metal corrosion is achieved, such as amines, heterocyclic compounds and imidazoles. The natural plant extracts mainly include compounds extracted from roots, stems, leaves, flowers, seeds, and fruit skins of natural plants. The composite corrosion inhibitor is formed by mixing two or more corrosion inhibitors, and the corrosion inhibition efficiency after the composite corrosion inhibitor is compounded is obviously improved due to the synergistic effect of the corrosion inhibitors. The corrosion inhibitor is a metal corrosion prevention technology with low investment, quick response, strong universality and simple and easy operation, and is widely applied to the field of metal corrosion protection. However, the conventional corrosion inhibitor is easy to lose, inactivate, hydrolyze or degrade in a corrosion medium, and in addition, the conventional corrosion inhibitor is mostly added in a one-time or continuous timing manner, so that the corrosion inhibitor cannot be accurately added according to the actual corrosion condition, and the problems of short effective action period, low utilization rate, poor stability, insufficient corrosion inhibition performance and the like of the corrosion inhibitor exist, so that a large amount of corrosion inhibition chemicals are wasted, and environmental pollution is caused.
In summary, the problems of the prior art are as follows: because the conventional corrosion inhibitor is easy to lose, inactivate, hydrolyze or degrade in a corrosion medium, and the conventional corrosion inhibitor is mostly added in a one-time or continuous timing manner, so that the conventional corrosion inhibitor cannot be accurately added according to the actual corrosion condition, and the problems of short effective action period, low utilization rate, poor stability, insufficient corrosion inhibition performance and the like of the corrosion inhibitor exist all the time, so that a large amount of corrosion inhibition agents are wasted, and the environmental pollution is caused.
Disclosure of Invention
The invention provides a pH value response intelligent control release corrosion inhibitor and a preparation method thereof, aiming at the problems of the prior conventional corrosion inhibitor technology. According to the characteristic that the pH value of a corrosion medium is increased when metal is corroded in the corrosion medium, a corrosion inhibition agent is wrapped by a pH value sensitive material to prepare a corrosion inhibition capsule, and when the capsule is stimulated by the change of the pH value caused by metal corrosion, the corrosion inhibition agent is quickly released, so that the metal corrosion is effectively inhibited, the loss, hydrolysis and degradation of the corrosion inhibitor are effectively prevented, the utilization rate of the corrosion inhibitor is improved, and the defects of the traditional corrosion inhibitor are overcome.
The invention is realized in such a way that a pH value response intelligent control release corrosion inhibitor consists of a novel anionic pH value sensitive material and a corrosion-retarding medicament Benzotriazole (BTA); the corrosion inhibitor BTA is wrapped by a pH value sensitive material, when the metal material is corroded, the pH value of the environment is increased, the capsule is swelled, and the corrosion inhibitor is released to effectively inhibit the metal corrosion.
Further, the molecular structural formula of the pH response capsule is as follows:
the corrosion inhibitor is Benzotriazole (BTA), and the molecular structural formula is as follows:
the invention also aims to provide a preparation method of the pH value response intelligent control release corrosion inhibitor, which comprises the following steps:
adding 2.1-4.8 g of vinyl triethoxysilane and 30-90 mL of ethylene glycol monomethyl ether into a 250mL three-necked flask, installing a mechanical stirrer, starting stirring, heating the flask to 60-85 ℃ in an oil bath, introducing nitrogen, and adding 0.02-0.12 g of initiator azobisisobutyronitrile and 3.5-7.5 g of corrosion inhibitor BTA;
and (2) continuously stirring, gradually dropwise adding 4.8-13.0 g of acrylic acid and 3.5-6.7 g of octadecyl acrylate into the reaction solution through a constant-pressure funnel for 2 hours, then stirring and reacting for 2-5 hours at the temperature of 60-85 ℃, then adding 0.1-0.6 g of N, N' -dimethylene bisacrylamide, continuously stirring and reacting for 1-3 hours to obtain a viscous polymer, adding 1.5-3.5 g of polyethylene imine (PET), and stirring and reacting for 0.5-2.0 hours to obtain the corrosion inhibition capsule.
And taking out the obtained viscous polymer, putting the viscous polymer into a watch glass, and performing forced air drying at 40-90 ℃ to remove the ethylene glycol monomethyl ether solvent to obtain the pH value response intelligent control release corrosion inhibitor.
The invention has the advantages and positive effects that:
the existing corrosion inhibitor has the defect of easy loss, the corrosion of materials is often accompanied by the change of pH value, at the moment, the intelligent corrosion inhibition capsule is controlled by the pH value response to start to release a corrosion inhibition medicament, so that the corrosion of the materials is prevented, the 'adding as required' of the corrosion inhibition medicament is realized, the corrosion protection time of the corrosion inhibitor is prolonged, and the defect that the corrosion inhibitor is easy to lose can be effectively solved.
1. The invention synthesizes a pH value sensitive type high polymer material capable of responding under an alkaline condition, a corrosion inhibitor BTA is wrapped by the material to prepare a pH value intelligent corrosion inhibition capsule, the capsule can start responding when the pH value is more than or equal to 7.0, a large amount of corrosion inhibitors are released, the pH value of Q235 steel is just increased slowly from 7.0 when the Q235 steel is corroded in seawater, the pH value is consistent with the response pH value of the corrosion inhibition capsule, and the 'adding according to the requirement' and the 'accurate corrosion inhibition' of the corrosion inhibitors in seawater medium of the Q235 steel can be realized.
2. The BTA corrosion inhibitor capsule has obvious effects on reducing the consumption of the corrosion inhibitor, improving the utilization rate of the corrosion inhibitor, reducing the adding times and the like, for example, when the BTA corrosion inhibitor is used for inhibiting the corrosion behavior of Q235 steel in simulated seawater, the corrosion inhibition efficiency of the BTA corrosion inhibitor capsule reaches 95.6% in 240h, the consumption of the BTA corrosion inhibitor capsule is reduced by 75.9% compared with the single BTA corrosion inhibitor, the BTA corrosion inhibitor capsule only needs to be added once, and the single BTA corrosion inhibitor needs to be added for more than 3 times to achieve the same corrosion inhibition effect.
3. The invention expands the application field of the conventional corrosion inhibitor. The uncured corrosion inhibition capsules are doped into the epoxy resin coating (the mass ratio of the two is 3:7) to prepare the metal material epoxy corrosion inhibition coating, when a metal substrate is corroded, the corrosion inhibitor wrapped in the corrosion inhibition capsules is released to inhibit metal corrosion, so that the service life of the epoxy anticorrosion coating can be prolonged by more than 2 times, the corrosion inhibition efficiency reaches 98.9%, the cost is reduced by more than 50.0%, and the application field of the corrosion inhibitor is further expanded.
Drawings
FIG. 1 is a flow chart of a method for preparing a pH-responsive intelligent controlled release corrosion inhibitor according to an embodiment of the present invention.
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.
The following detailed description of the principles of the invention is provided in connection with the accompanying drawings.
The pH response intelligent control release corrosion inhibitor provided by the embodiment of the invention consists of a pH response capsule and a corrosion inhibitor, wherein the corrosion inhibitor is wrapped by the pH response capsule, when the material is corroded, the pH of the environment is increased, and at the moment, the capsule is swelled, the corrosion inhibitor is released, and the material corrosion is effectively prevented.
As shown in fig. 1, the preparation method of the pH-responsive intelligent controlled release corrosion inhibitor provided by the embodiment of the present invention includes:
s101: adding 2.1-4.8 g of vinyl triethoxysilane and 30-90 mL of ethylene glycol monomethyl ether into a 250mL three-necked flask, installing a mechanical stirrer, starting stirring, heating in an oil bath to 60-85 ℃, introducing nitrogen, adding 0.02-0.12 g of initiator azodiisobutyronitrile and 3.5-7.5 g of corrosion inhibitor Benzotriazole (BTA);
s102: and (2) continuously stirring, gradually dropwise adding 4.8-13.0 g of acrylic acid and 3.5-6.7 g of octadecyl acrylate into the reaction solution through a constant-pressure funnel for 2 hours, then stirring and reacting for 2-5 hours at the temperature of 60-85 ℃, adding 0.1-0.6 g of N, N-dimethylene bisacrylamide, continuously stirring and reacting for 1-3 hours to obtain a viscous polymer, adding 1.5-3.5 g of polyethyleneimine, and stirring and reacting for 0.5-2.0 hours to obtain the corrosion inhibition capsule.
S103: and taking out the obtained viscous polymer, putting the viscous polymer into a watch glass, and performing forced air drying at 40-90 ℃ to remove the ethylene glycol monomethyl ether solvent to obtain the pH value response intelligent control release corrosion inhibitor.
The molecular synthesis process and the molecular structural formula of the pH value response intelligent control release corrosion inhibition capsule provided by the embodiment of the invention are as follows:
the corrosion inhibition agent is Benzotriazole (BTA):
the invention is further described with reference to specific examples.
Example 1:
adding 3.0g of vinyl triethoxysilane and 60mL of ethylene glycol monomethyl ether into a 250mL three-neck flask, installing a mechanical stirrer, starting stirring, heating in an oil bath to 70 ℃, introducing nitrogen, adding 0.06g of initiator azobisisobutyronitrile and 5.0g of corrosion inhibitor Benzotriazole (BTA);
and (2) continuously stirring, gradually dropwise adding 9.0g of acrylic acid and 6.0g of octadecyl acrylate into the reaction solution through a constant-pressure funnel, completing the dropwise addition within 2h, then stirring and reacting for 2h at 75 ℃, then adding 0.3g of N, N-dimethylene bisacrylamide, continuously stirring and reacting for 1h to obtain a viscous polymer, adding 2.0g of Polyethyleneimine (PEI), and stirring and reacting for 1h to obtain the corrosion inhibition capsule.
And taking out the obtained viscous polymer, putting the viscous polymer into a watch glass, and performing forced air drying at the temperature of 60 ℃ to remove the solvent ethylene glycol monomethyl ether to obtain the pH value response intelligent control release corrosion inhibitor.
Example 2:
adding 5.5g of octadecyl acrylate and 70mL of ethylene glycol methyl ether into a 250mL three-neck flask, installing a mechanical stirrer, starting stirring, heating the mixture to 70 ℃ in an oil bath, introducing nitrogen, adding 0.08g of initiator azodiisobutyronitrile and 6.0g of corrosion inhibitor Benzotriazole (BTA);
stirring is continued, 11.0g of acrylic acid and 3.6g of vinyl triethoxysilane are gradually dripped into the reaction solution through a constant pressure funnel, after dripping is finished within 2h, stirring reaction is carried out for 3h at 75 ℃, then 0.2g of N, N-dimethylene bisacrylamide is added, stirring reaction is continued for 2h to obtain a viscous polymer, 1.5g of Polyethyleneimine (PEI) is added, and stirring reaction is carried out for 0.5h to obtain the corrosion inhibition capsule.
And taking out the obtained viscous polymer, putting the viscous polymer into a watch glass, and performing forced air drying at 50 ℃ to remove the solvent ethylene glycol monomethyl ether to obtain the pH value response intelligent control release corrosion inhibitor.
Example 3:
adding 7.0g of acrylic acid and 50mL of ethylene glycol monomethyl ether into a 250mL three-neck flask, installing a mechanical stirrer, starting stirring, heating the mixture to 70 ℃ in an oil bath, introducing nitrogen, and adding 0.10g of initiator azobisisobutyronitrile and 5.5g of corrosion inhibitor;
stirring is continued, 4.8g of vinyltriethoxysilane and 6.7g of octadecyl acrylate are gradually dripped into the reaction solution through a constant pressure funnel, after dripping is finished within 2h, stirring reaction is carried out for 3h at 70 ℃, then 0.5g of N, N-dimethylene bisacrylamide is added, stirring reaction is continued for 3h to obtain a viscous polymer, 3.0g of Polyethyleneimine (PEI) is added, and stirring reaction is carried out for 1.5h to obtain the corrosion inhibition capsule.
And taking out the obtained viscous polymer, putting the viscous polymer into a watch glass, and performing forced air drying at 70 ℃ to remove the ethylene glycol monomethyl ether solvent to obtain the pH value response intelligent control release corrosion inhibitor.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (2)
1. A pH value response intelligent control release corrosion inhibition capsule is characterized in that the pH value response intelligent control release corrosion inhibition capsule is wrapped by a pH sensitive capsule, when a metal material is corroded, the pH value of the environment can be increased, and when the pH value is more than or equal to 7.0, a corrosion inhibition medicament can be quickly released from the capsule to inhibit the corrosion of the metal material; the pH value response intelligent control release corrosion inhibitor consists of 65-85% of pH response capsules and 15-35% of corrosion inhibition medicaments according to mass fraction;
the preparation process of the pH response intelligent corrosion inhibition capsule is shown as follows:
the wrapped corrosion inhibition agent is benzotriazole, and the molecular formula is as follows:
the preparation method of the pH value response intelligent control release corrosion inhibitor comprises the following steps:
adding 2.1-4.8 g of vinyl triethoxysilane and 30-90 mL of ethylene glycol monomethyl ether into a 250mL three-necked flask, installing a mechanical stirrer, starting stirring, heating in an oil bath to 60-85 ℃, introducing nitrogen, and adding 0.02-0.12 g of initiator azobisisobutyronitrile and 3.5-7.5 g of corrosion inhibitor;
continuously stirring, gradually dripping 4.8-13.0 g of acrylic acid and 3.5-6.7 g of octadecyl acrylate into the reaction solution through a constant pressure funnel within 2 hours, then stirring and reacting for 2-5 hours at the temperature of 60-85 ℃, then adding 0.1-0.6 g N, N' -dimethylene bisacrylamide, continuously stirring and reacting for 1-3 hours to obtain a viscous polymer, adding 1.5-3.5 g of polyethyleneimine, and stirring and reacting for 0.5-2.0 hours to obtain a corrosion inhibition capsule;
and taking out the obtained viscous polymer, putting the viscous polymer into a watch glass, and performing forced air drying at 40-90 ℃ to remove the ethylene glycol monomethyl ether solvent to obtain the pH value response intelligent control release corrosion inhibitor.
2. Use of the pH responsive intelligent controlled release corrosion inhibiting capsule of claim 1 in seawater.
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| CN103031559B (en) * | 2013-01-06 | 2015-06-24 | 北京科技大学 | Preparation of pH-controlled-release long-acting intelligent corrosion inhibitor |
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