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Preparation method of polythioether corrosion inhibitor containing cobaltocene cation side group and used corrosion inhibitor system

A technology of cobaltene cation and polysulfide, which can be used in coatings, anti-corrosion coatings, etc., and can solve the problems of poor film-forming ability and few attachment sites of small-molecule corrosion inhibitors

Active Publication Date: 2021-12-31
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to avoid the deficiencies of the prior art, the present invention proposes a preparation method of a polysulfide corrosion inhibitor containing dicyclocene cobalt cationic side groups and a corrosion inhibitor system, in order to provide a kind of corrosion inhibitor through a convenient and efficient synthesis method. The polysulfide corrosion inhibitor containing dicyclocobaltium ion side groups and its use method aims to solve the shortcomings of small molecule corrosion inhibitors such as poor film-forming ability and few attachment sites, and develop new polymer corrosion inhibitors

Method used

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  • Preparation method of polythioether corrosion inhibitor containing cobaltocene cation side group and used corrosion inhibitor system
  • Preparation method of polythioether corrosion inhibitor containing cobaltocene cation side group and used corrosion inhibitor system
  • Preparation method of polythioether corrosion inhibitor containing cobaltocene cation side group and used corrosion inhibitor system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1: When X - = Cl - When the preparation of structural formula 1

[0044] Dissolve 1,6-heptadien-4-ol in an appropriate amount of dichloromethane, add 1-3 parts of triethylamine, 2-6 parts of methanesulfonic anhydride, 0.5-1 parts 4-Dimethylaminopyridine, low temperature reaction 1-4h, room temperature reaction 24-48h. Add water to quench the reaction, add an equal amount of dichloromethane for extraction and separation, remove the organic phase, and obtain 1,6-heptadiene-4-methylsulfonate through column separation and purification.

[0045] Put 1 part of 1,6-heptadiene-4-methylsulfonate and 1 part of octanedithiol in a vial, add 0.01-0.05 part of photoinitiator, and irradiate with 365nm ultraviolet light for 0.5-2h. The product was dissolved in tetrahydrofuran and precipitated twice in methanol to obtain a polythioether containing methylsulfonate side groups.

[0046] Dissolve the polythioether containing methylsulfonate side groups in a small amount of N,N-...

Embodiment 2

[0049] Example 2: When X - = Cl - When the preparation of structural formula 2

[0050] Dissolve 1-3 parts of allyl bromide, 1-5 parts of potassium iodide and 1-3 parts of stannous chloride hydrate in 10-30mL water and place in a round bottom flask, and dissolve 1-3 parts of glyoxal in 5 -10mL water and dropwise into the above round bottom flask, react at room temperature for 24-48h, add 5-20mL 1M HCl solution, add ethyl acetate for extraction and separation three times, add appropriate amount of sodium thiosulfate hydrate for decolorization, and then use Ethyl acetate was extracted and separated once, and the organic phase was removed and dried to obtain 1,7-octadiene-4,5-diol.

[0051] Dissolve 1,7-octadiene-4,5-diol in an appropriate amount of dichloromethane, add 1-3 parts of triethylamine, 2-6 parts of methanesulfonic anhydride, 0.5 - 1 part of 4-dimethylaminopyridine, react at low temperature for 1-4h, and at room temperature for 24-48h. Add water to quench the react...

Embodiment 3

[0056] Example 3: When X - = Cl - When the preparation of structural formula 3

[0057] Dissolve 1 part of diethyl diallylmalonate in 5-15 mL of ether and place in a round bottom flask, disperse 1-3 parts of lithium aluminum hydride in 10-20 mL of ether and slowly add the above In a round bottom flask, stir at room temperature for 12-24h. Add an appropriate amount of water to quench the reaction, filter to remove the precipitate, add an appropriate amount of dichloromethane for multiple extractions, remove the organic phase, and dry to obtain diallyl propylene glycol.

[0058] Dissolve diallyl propylene glycol in an appropriate amount of dichloromethane, add 1-3 parts of triethylamine, 2-6 parts of methanesulfonic anhydride, and 0.5-1 part of 4-dimethylaminopyridine in a nitrogen atmosphere and ice bath , low temperature reaction 1-4h, room temperature reaction 24-48h. Water was added to quench the reaction, an equal amount of dichloromethane was added to extract and separ...

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Abstract

The invention relates to a preparation method of a polythioether corrosion inhibitor containing a cobaltocene cation side group and a used corrosion inhibitor system. Through an ingenious structural design, sulfur atoms are introduced into a polymer main chain by utilizing a simple and convenient thiol-ene click polymerization reaction to obtain saturated polythioether of which the side chain contains sulfonate groups with different numbers; and the target polythioether corrosion inhibitor of which the side chain contains different numbers of cobaltocene onium ions is prepared through efficient azidation and copper-catalyzed azide-alkynyl click reaction. According to the polymer corrosion inhibitor, the interaction between the corrosion inhibitor and the metal surface can be further enhanced through the synergistic effect of sulfur atoms on a main chain, side group connecting groups of triazole and cobaltocene onium ions and the metal surface and the excellent film-forming property of the polymer, so that the excellent corrosion inhibition effect is achieved. The final corrosion inhibition experiment test shows that when the corrosion inhibitor is immersed in a 5% HCl corrosion inhibition medium for 6 hours at the temperature of 25 DEG C, the corrosion inhibition efficiency of the corrosion inhibitor with the concentration of 15 ppm on metal reaches up to 96%.

Description

technical field [0001] The invention belongs to the field of chemical anti-corrosion, and relates to a preparation method of a polysulfide corrosion inhibitor containing cobaltocene cation side groups and a corrosion inhibitor system. Background technique [0002] Metal corrosion is a major concern in most industrialized countries. Corrosion-related maintenance costs in industrial facilities in many countries have been reported to represent 1–5% of their gross national product. A study published by the National Association of Corrosion Engineering in 2013 showed that the global cost of corrosion was estimated at $2.5 trillion, equivalent to 3.4% of the global gross domestic product for that year. What's more, once the infrastructure collapses, corrosion can cause loss of economy, natural resources, and human life, so it is crucial to study mature corrosion mitigation technologies. The current corrosion mitigation methods include anodic protection, cathodic protection, coat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/045C09D5/08C09D181/02
CPCC08G75/045C09D5/08C09D181/02
Inventor 闫毅刘爽颜静蔡宁静石朝阳张军平
Owner NORTHWESTERN POLYTECHNICAL UNIV
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