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Synthesis method of inert end group polythioether polymer

A technology of terminal polythioether and synthesis method, which is applied in the field of synthesis of inert terminal polythioether polymers, can solve the problems of poor temperature resistance, poor compatibility and easy precipitation, etc., to improve comprehensive performance, reaction Stable and good temperature resistance

Pending Publication Date: 2021-03-02
锦西化工研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Plasticizers are the main additives for the preparation of polythioether sealants, which can reduce the viscosity of the sealant and improve the construction performance of the sealant. At present, the commonly used polythioether plasticizers include butyl benzyl phthalate, epoxy Soybean oil, triphenyl phosphate, etc. have problems such as poor temperature resistance, poor compatibility with polythioether rubber and easy precipitation

Method used

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  • Synthesis method of inert end group polythioether polymer
  • Synthesis method of inert end group polythioether polymer
  • Synthesis method of inert end group polythioether polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 500ml three-necked flask equipped with a stirrer and a thermometer, add 150 g of mercaptoethanol (industrial product, purity 99%), 2.25 g of tert-butyl peroxybenzoate, 0.23 g of tetramethylguanidine, and dropwise add styrene (industrial product , purity 99%) 174g, heat up to 80°C ± 2°C, react for 7 hours, control the crude product kettle temperature at 130°C ~ 160°C, and rectify below the residual pressure of 2.66kPa to obtain 1-hydroxyl-3-thia-5 -Phenylpentane, yellowish in color and 98% pure, figure 1 It is the infrared spectrum of 1-hydroxy-3-thia-5-phenylpentane.

[0026] In a 500ml three-necked flask equipped with a stirrer and a thermometer, add thiodiglycol (industrial product, purity 98%) 150g, 1-hydroxyl-3-thia-5-phenylpentane (purity 98%) 63.8 g, triphenyl phosphite 2.25, heat up to 160°C ± 2°C, after 8 hours of reaction, the reaction product needs to be extracted by solvent to remove unreacted small molecules, and the residual pressure is below 2.66kPa ...

Embodiment 2

[0028] 1-Hydroxy-3-thia-5-phenylpentane was synthesized by the method in Example 1.

[0029] In a 500ml three-necked flask equipped with a stirrer and a thermometer, add thiodiglycol (industrial product, purity 98%) 150g, 1-hydroxy-3-thia-5-phenylpentane (purity 98%) 54.7 g, triphenyl phosphite 2.25, heat up to 125°C ± 2°C, after 9 hours of reaction, the reaction product needs to be extracted by solvent to remove unreacted small molecules, and the residual pressure is below 2.66kPa to carry out vacuum reaction for 2h to obtain the inert end Polythioether-based polymer, light yellow in color, 0.1% moisture, 0.15 mg acid value, 1.17 g / cm3 relative density, and 660 (25°C) mPa·s viscosity.

Embodiment 3

[0031] 1-Hydroxy-3-thia-5-phenylpentane was synthesized by the method in Example 1.

[0032] In a 500ml three-necked flask equipped with a stirrer and a thermometer, add thiodiglycol (industrial product, purity 98%) 150g, 1-hydroxyl-3-thia-5-phenylpentane (purity 98%) 74.1 g, triphenyl phosphite 2.25, heat up to 180°C±2°C, after 6 hours of reaction, the reaction product needs to be extracted by solvent to remove unreacted small molecules, and the residual pressure is below 2.66kPa for vacuum reaction for 2h to obtain the inert end based polythioether polymers. The color is light yellow, the water content is 0.1%, the acid value is 0.15 mg, the relative density is 1.17 g / cm3, and the viscosity is 350 (25°C) mPa·s.

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Abstract

The invention discloses a synthesis method of an inert end group polythioether polymer, which comprises the following steps of: (1) mixing raw materials styrene and mercaptoethanol according to a molar ratio of 1: (1-1.3), adding a catalyst A, reacting under heating conditions to generate a 1-hydroxy-3-thia-5-phenyl pentane crude product, and rectifying the crude product to obtain 1-hydroxy- 3-thia-5-phenyl pentane; (2) mixing the 1-hydroxy-3-thia-5-phenyl pentane obtained by rectification with thiodiethylene glycol according to a molar ratio of 1: (3.0-4.5), adding a catalyst B, and then heating to carry out a hydroxyl dehydration polycondensation reaction; and (3) after solvent extraction, removing low-boiling-point substances under a vacuum heating condition to obtain the inert end group polythioether polymer. The problem that an existing plasticizer for a polythioether sealant is poor in temperature resistance, poor in compatibility and the like is solved, the comprehensive performance of the sealant is improved, and the used raw materials are cheap, easy to obtain and stable in reaction.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a method for synthesizing an inert terminal polythioether polymer. Background technique [0002] Polythioether is a kind of aliphatic saturated polymer containing monosulfide bonds in the main chain of the molecule. The sealant formulated with polythioether as the base polymer has high and low temperature resistance, fuel resistance, solvent resistance, water resistance, weather resistance, etc. Excellent performance, can be vulcanized at low temperature or heat, which meets the sealing of the overall fuel tank of the aircraft and its low-temperature quick repair, pressure cabin, flap system, fairing, and electrical equipment. Plasticizers are the main additives for the preparation of polythioether sealants, which can reduce the viscosity of the sealant and improve the construction performance of the sealant. At present, the commonly used polythioether plast...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/025
CPCC08G75/0272
Inventor 赫平杨菲刘浩然
Owner 锦西化工研究院有限公司
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