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A kind of polythioether-based polythiol, its synthesis method and application

A synthesis method and technology of polysulfide, applied in the preparation of sulfide, organic chemistry, etc., can solve the problems of limited ability to block corrosion medium and low thickness, and achieve the effect of strong adhesion, high density and high thickness

Active Publication Date: 2017-01-25
宁波海强装备科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the thickness of these three films is generally low, all less than 100nm, resulting in limited ability to block corrosive media

Method used

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  • A kind of polythioether-based polythiol, its synthesis method and application
  • A kind of polythioether-based polythiol, its synthesis method and application
  • A kind of polythioether-based polythiol, its synthesis method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In this embodiment, the structural formula of polythioether-based polythiol is:

[0030]

[0031] The preparation method of above-mentioned polythioether-based polythiol comprises the steps:

[0032] (1) Add 1 mole part of ethanedithiol, 0.9 mole part of propynyl thioacetate, and 0.01 mole part of azobisisobutyronitrile in the reactor, and carry out mercapto-alkyne reaction at 70°C. Addition polymerization reaction 0.5 hour;

[0033] (2) Under the protection of nitrogen, the product obtained in step (1) was dissolved in 0.25 molar parts of ethanol, followed by adding 0.01 molar parts of water and 0.01 molar parts of hydrochloric acid, and hydrolyzed at 50 ° C for 24 hours;

[0034] (3) The product obtained in step (2) is evaporated to remove ethanol, and the polythioether-based polythiol is obtained through precipitation and drying.

[0035] figure 1 It is the product obtained in the above step (1) 1 H NMR spectrum. figure 2 Be the polythioether group polythiol...

Embodiment 2

[0038] In this embodiment, the structural formula of polythioether-based polythiol is:

[0039]

[0040] The preparation method of above-mentioned polythioether-based polythiol comprises the steps:

[0041] (1) Add 1 mole part of ethanedithiol compound, 1 mole part of propynyl thioacetate, and 0.1 mole part of azobiscyanovaleric acid in sequence in the reactor, and carry out mercapto reaction at 50°C. - Alkyne addition polymerization reaction for 24 hours;

[0042] (2) Under nitrogen protection, dissolve the product obtained in step 1) in 10 moles of toluene, add 1 moles of methanol and 0.1 moles of p-toluenesulfonic acid in turn, and react at 120° C. for 1 hour;

[0043] (3) The product obtained in step (2) is evaporated to remove the solvent, and the polythioether-based polythiol is obtained through precipitation and drying.

[0044] Same as Example 1, the molecular side chain of the polythioether-based polythiol prepared above contains a large amount of mercapto groups, ...

Embodiment 3

[0046] In this embodiment, the structural formula of polythioether-based polythiol is:

[0047]

[0048] The preparation method of above-mentioned polythioether-based polythiol comprises the steps:

[0049] (1) Add 1 mole part of propanedithiol, 0.95 mole part of butynyl thioacetate, and 0.05 mole part of azobisisobutyronitrile in the reactor, and carry out mercapto-alkyne reaction at 65°C. Addition polymerization reaction for 12 hours;

[0050] (2) Under the protection of nitrogen, dissolve the product obtained in step 1) in 1 mole part of tetrahydrofuran, add 0.1 mole part of water and 0.02 mole part of hydrochloric acid in sequence, and react at 65 ° C for 12 hours;

[0051] (3) The product obtained in step (2) is evaporated to remove the solvent, and the polythioether-based polythiol is obtained through precipitation and drying.

[0052] Same as Example 1, the molecular side chain of the polythioether-based polythiol prepared above contains a large amount of mercapto ...

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Abstract

The invention provides a polythioether-base compound, of which the side chain structure contains abundant mercapto group, thereby forming the polythioether-base polymercaptan. The invention also provides a method for synthesizing the polythioether-base polymercaptan, which comprises the following steps: carrying out mercapto-alkyne addition polymerization reaction to obtain polythioether, and carrying out acidic hydrolysis. The method has the advantages of high speed, high efficiency, simple technique and high yield. The mercapto group in the polythioether-base polymercaptan molecular chain can form a sulfur-copper bond with copper, the mercaptan bond can be self-condensed to form a compact thick-film coating, and thus, the polythioether-base polymercaptan can be used as a copper corrosion inhibitor. The slow-release film formed by the polythioether-base polymercaptan on the copper surface has the advantages of high adhesion, high compactness and high thickness, satisfies the performance requirements on the copper corrosion inhibition film at present, and effectively protects the copper base from external corrosion.

Description

technical field [0001] The invention relates to a polythioether-based compound, in particular to a polythioether-based polythiol, its synthesis method and application. Background technique [0002] Copper has excellent strength, machinability, electrical conductivity, and thermal conductivity, and is widely used in electrical, light industry, machinery manufacturing, construction industry, defense industry and other fields. However, copper corrodes in the atmosphere, oxygenated water, oxidizing acids, and electrolyte solutions. Therefore, the anti-corrosion protection of copper is one of the important factors to maintain its stable performance. [0003] There are many anti-corrosion technologies, such as: cathodic protection, organic coating protection, corrosion inhibitors, etc. Among them, the corrosion inhibitor refers to the addition of a small amount or a small amount of such chemical substances in the medium, which can greatly reduce the corrosion rate of the metal i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/045C08G75/12C07C321/14C07C323/12C07C319/20C23F11/173
Inventor 王刚韩金顾凌晓彭叔森乌学东
Owner 宁波海强装备科技有限公司