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A metal passivator for preventing corrosive sulfur corrosion and its preparation method and application

A metal passivator and corrosive sulfur technology, which is applied in metal material coating technology, additives, organic chemistry and other directions, can solve the problems of high toxicity of aquatic organisms, poor treatment effect of adsorbents, and high cost of new adsorbents. Low cost, simple preparation method, and the effect of improving safety

Inactive Publication Date: 2019-04-16
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The regeneration technology of insulating oil is to use adsorbents to adsorb polar substances such as corrosive sulfur. However, due to the poor treatment effect of traditional adsorbents and the high cost of new adsorbents, this method is rarely used in practice; another method It is to add a benzotriazole metal passivator to the insulating oil. The metal passivator reacts with the conductor copper to form a passivation film on its surface, thereby preventing the corrosion of the copper surface by corrosive sulfur. This method is relatively low in cost , easy to operate, has been widely used
[0005] The widely used benzotriazole metal deactivator is commercial Irgamet39 TM , the product has good oil solubility and good anti-corrosion effect, but the product is highly toxic to aquatic organisms

Method used

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  • A metal passivator for preventing corrosive sulfur corrosion and its preparation method and application
  • A metal passivator for preventing corrosive sulfur corrosion and its preparation method and application
  • A metal passivator for preventing corrosive sulfur corrosion and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0025] In the present embodiment 1, hemiacetal group benzoxazole metal deactivator, structure is as follows:

[0026]

[0027] The preparation method of above-mentioned metal deactivator, comprises the steps:

[0028] 11.9g of benzotriazole, 132g of dioxane, 31.5g of tert-butanol peroxide and 0.32g of tetrabutylammonium iodide were dissolved in 400mL of dichloroethane, and then the mixture was heated to reflux, and after the reaction was detected by TLC . After the solvent was evaporated, it was extracted with ethyl acetate, and the product was separated by column chromatography in an ethyl acetate-n-hexane system. The structure of the compound was confirmed by nuclear magnetic spectrum. 1 H NMR (400MHz, CDCl 3 )δ8.09(d, J=8.3Hz, 1H), 7.76(d, J=8.3Hz, 1H), 7.53(t, J=7.6Hz, 1H), 7.40(t, J=7.6Hz, 1H) , 6.10(dd, J=7.2, 2.8Hz, 1H), 4.54(dd, J=11.8, 7.3Hz, 1H), 4.24(dd, J=11.9, 2.7Hz, 1H), 4.03-3.80(m, 4H ); 13 C NMR (100MHz, CDCl 3 )δ146.0, 132.5, 127.9, 124.4, 120.1, 11...

Embodiment 2

[0030] In the present embodiment 2, hemiacetal group benzoxazole metal deactivator, structure is as follows:

[0031]

[0032] The preparation method of above-mentioned metal deactivator, comprises the steps:

[0033] 11.9 g of benzotriazole, 108 g of tetrahydrofuran, 31.5 g of tert-butanol peroxide and 0.32 g of tetrabutylammonium iodide were dissolved in 400 mL of dichloroethane, then the mixture was heated to reflux, TLC detected that the reaction was complete, and after the solvent evaporated It is extracted with ethyl acetate, and the product is separated by column chromatography through ethyl acetate-n-hexane system. The structure of the compound was confirmed by nuclear magnetic spectrum. 1 H NMR (400MHz, CDCl 3 )δ: 7.99(d, J=8.3Hz, 1H), 7.64(d, J=8.3Hz, 1H), 7.43(t, J=7.6Hz, 1H), 7.31(t, J=7.6Hz, 1H) , 6.44(dd, J=6.5, 1.6Hz, 1H), 4.10-3.88(m, 2H), 3.20-3.10(m, 1H), 2.57-2.47(m, 1H), 2.32-2.43(m, 1H) , 2.19-2.04(m, 1H); 13 C NMR (100.61 MHz, CDCl 3 )δ146.2, 132...

Embodiment 3

[0035] In the present embodiment 3, hemiacetal group benzoxazole metal deactivator, structure is as follows:

[0036]

[0037] The preparation method of above-mentioned metal deactivator, comprises the steps:

[0038] Benzotriazole 11.9g, tetrahydropyran 129g, tert-butanol peroxide 31.5g and tetrabutylammonium iodide 0.32g were dissolved in 400mL of dichloroethane, then the mixture was heated to reflux, and TLC detected that the reaction was complete. After the solvent was evaporated, it was extracted with ethyl acetate, and the product was separated by column chromatography in an ethyl acetate-n-hexane system. The structure of the compound was confirmed by nuclear magnetic spectrum. 1 H NMR (400MHz, CDCl 3 )δ8.08(d, J=8.4Hz, 1H), 7.75(d, J=8.3Hz, 1H), 7.50(t, J=7.6Hz, 1H), 7.39(t, J=7.6Hz, 1H) , 6.05(dd, J=8.2, 2.8Hz, 1H), 3.96(dd, J=11.6, 4.4Hz, 1H), 3.86-3.72(m, 1H), 2.71-2.56(m, 1H), 2.29-2.11 (m, 2H), 1.87-1.68 (m, 3H); 13 C NMR (100MHz, CDCl 3 )δ146.2, 132.5, 12...

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Abstract

The invention relates to a metal deactivator used for preventing corrosive sulfur corrosion, and a preparation method and applications thereof. The metal deactivator is a hemiacetal benzoxazole compound with a structure represented by formula I, wherein R1 and R2 are respectively selected from H or Me at random, A is selected from N or CH at random, n is equal to 1 or 2, X is selected from CH2 or O at random. No high toxicity substances including formaldehyde and bis(2-ethylhexyl)amine is released into the environment in application process of the metal deactivator, additive utilization safety is improved, and the metal deactivator can be widely applied in electrical equipment such as power transformers, distribution transformers, or electric reactors.

Description

technical field [0001] The invention relates to the technical field of preventing corrosive sulfur for transformers, in particular to a metal passivator for preventing corrosive sulfur corrosion and its preparation method and application. Background technique [0002] Insulating oil-solid insulating paper insulation system is widely used in power transformers, distribution transformers and reactors due to its low price and good performance. The dielectric strength of this system is strongly dependent on its insulation properties. [0003] At present, some insulating oils contain corrosive sulfur, which chemically reacts with the copper conductor of the transformer to form cuprous sulfide with poor insulation performance. The generation of cuprous sulfide will reduce the initial partial discharge level. Under high field strength or transient current, partial discharge will degrade the solid insulating paper and cause failure. In extreme cases, a large amount of cuprous sulfi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D405/04C10M133/44C10M133/46C23C22/02C10N40/16C10N30/12
CPCC07D405/04C10M133/44C10M133/46C10M2215/223C10M2215/224C10N2030/12C10N2040/16C23C22/02
Inventor 赵耀洪钱艺华苏伟张丽钟力生于钦学李亚飞
Owner XI AN JIAOTONG UNIV