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Synthetic method for epoxy end group polythioether liquid rubber

A technology based on polythioether and liquid rubber, which is applied in the field of high molecular polymer production, can solve the problem of severe reaction heat release, etc., and achieve the effects of uniform molecular weight distribution, stable reaction, and easy product quality

Active Publication Date: 2015-04-29
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

Polyethylene glycol diglycidyl ether resin is used as the terminal conversion agent, which overcomes the disadvantages of excessive viscosity in the traditional process of mercapto epoxy modification, the need to add solvents such as toluene and methyl ethyl ketone to dilute, the reaction is exothermic, and side reactions are prone to occur. ; The reaction is stable, the product quality is easy to control, and the generated epoxy-terminated polythioether liquid rubber has moderate viscosity and uniform molecular weight distribution

Method used

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  • Synthetic method for epoxy end group polythioether liquid rubber
  • Synthetic method for epoxy end group polythioether liquid rubber
  • Synthetic method for epoxy end group polythioether liquid rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 5L stainless steel reaction kettle equipped with a stirrer, a thermometer, a condenser, and a low-molecular receiver, put mercapto-terminated polythioether liquid rubber Ⅰ JLM-2006-4 (product of Jinxi Institute, number-average weight 3891, The degree of crosslinking is 2.5, the viscosity is 42.3Pa s) 4kg, 1.05kg polyethylene glycol diglycidyl ether resin (DER732), 11.6g peroxide and 1.4g amine composite catalyst, the temperature is raised to 80°C, and the reaction temperature is controlled 80±2℃, react for 12h, continue to heat up to 140℃, at 140±2℃, control the residual pressure below 20mmHg, carry out vacuum reaction for 4h, remove unreacted small molecular substances, and obtain epoxy-terminated polythioether liquid rubber Ⅱ, epoxy value 0.07, viscosity 62.5Pa·s, density 1.15g / cm 3 .

Embodiment 2

[0027] In a 5L stainless steel reaction kettle equipped with a stirrer, a thermometer, a condenser, and a low-molecular receiver, put mercapto-terminated polythioether liquid rubber Ⅰ JLM-2006-3 (product of Jinxi Institute, number-average weight 4217, The degree of crosslinking is 2.3, the viscosity is 45.8Pa s) 4kg, 0.9kg polyethylene glycol diglycidyl ether resin (DER732), 10.3g peroxide and 1.2g amine composite catalyst, the temperature is raised to 80°C, and the reaction temperature is controlled 80±2℃, react for 12h, continue to heat up to 140℃, at 140±2℃, control the residual pressure below 20mmHg, carry out vacuum reaction for 4h, remove unreacted small molecular substances, and obtain epoxy-terminated polythioether liquid rubber Ⅱ, epoxy value 0.06, viscosity 65.8Pa·s, density 1.15g / cm 3 .

Embodiment 3

[0029] In a 5L stainless steel reaction kettle equipped with a stirrer, a thermometer, a condenser, and a low-molecular receiver, put mercapto-terminated polythioether liquid rubber Ⅰ JLM-2006-1 (product of Jinxi Institute, number-average weight 4358, The degree of crosslinking is 2.8, the viscosity is 54.1Pa s) 4kg, 1.05kg polyethylene glycol diglycidyl ether resin (DER732), 11.6g peroxide and 1.4g amine composite catalyst, the temperature is raised to 80°C, and the reaction temperature is controlled 80±2℃, react for 12h, continue to heat up to 140℃, at 140±2℃, control the residual pressure below 20mmHg, carry out vacuum reaction for 4h, remove unreacted small molecular substances, and obtain epoxy-terminated polythioether liquid rubber Ⅱ, epoxy value 0.077, viscosity 70.5Pa·s, density 1.17g / cm 3 .

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Abstract

The invention discloses a synthetic method for epoxy end group polythioether liquid rubber. The method comprises the following steps: synthesizing sulphydryl end group polythioether liquid rubber by using thiodiglycol, hydroxyethyl-2-hydroxypropyl thioether and the like as main monomers; then using polyethylene glycol diglycidyl ether resin as a transforming agent so as to transform a sulphydryl end group into an epoxy end group so as to finally generate the end group polythioether liquid rubber. The technology has the advantages that the polyethylene glycol diglycidyl ether resin is adopted as the transforming agent of the end group, the defects that the viscosity of a sulphydryl in traditional epoxy modification technology is high, solvents of toluene, butanone and the like are needed to perform dilution, the reaction exotherm is violent, and a side effect is easy to generate are overcome; reactions are smooth, the product quality is easy to control, the viscosity of the generated epoxy end group polythioether liquid rubber is moderate, and the stability is good; the strength of epoxy resin and the toughness and the heat resistance of polythioether rubber are reserved after the end group is transformed, so that the brittleness of the epoxy resin is improved, and the adhesive property of materials is improved.

Description

technical field [0001] The invention belongs to the technical field of polymer production, and in particular relates to a synthesis method of epoxy-terminated polythioether liquid rubber. technical background [0002] Polythioether refers to a class of aliphatic saturated polymers containing monosulfide bonds in the main chain of the molecule. The sealant formulated based on polythioether has the performance of aging resistance and high temperature resistance that surpasses that of traditional polysulfide rubber sealants. 3 to 10 times, long-term use temperature range is -62 ℃ ~ 160 ℃, 216 ℃ short-term use, widely used in new aircraft supersonic cruise, low temperature repair, electrical and electronic materials, anti-corrosion materials, potting and casting materials and composite materials and other fields. [0003] Regarding the synthesis process of epoxy-terminated polythioether rubber, there are reports on epoxy-terminated polythioether and curable epoxy-terminated pol...

Claims

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Application Information

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IPC IPC(8): C08G65/48C08G81/00
Inventor 赫平王绍民马天野金慧明李锦
Owner 锦西化工研究院有限公司
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