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Epoxy terminated polysulfide rubber and its preparation and application

A polysulfide rubber and epoxy-terminated technology, used in adhesives, other chemical processes, chemical instruments and methods, etc., can solve the doubt of conversion rate and reactivity, difficulty in removing olefinic compounds, poor anti-aging performance, etc. problems, to achieve the effects of easy control of the reaction, fast reaction rate and simple preparation process

Active Publication Date: 2022-07-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this preparation method is obtained by the addition reaction of mercaptan in polysulfide rubber and epoxy-containing vinyl compounds under the action of compounds that can generate free radicals. The disadvantage is that there is an excessive amount of epoxy-containing compounds. It is difficult to remove olefinic compounds, and the residual olefinic compounds containing epoxy groups in the polymer will affect the aging resistance of the polymer due to double bonds after vulcanization and crosslinking, and the crosslinking density is low; in addition, mercaptans The conversion rate and reactivity of the addition reaction with double bonds are also questionable

Method used

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  • Epoxy terminated polysulfide rubber and its preparation and application
  • Epoxy terminated polysulfide rubber and its preparation and application
  • Epoxy terminated polysulfide rubber and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] The first step is to put 100g of JLY-121 polysulfide rubber (average molecular weight of 1000, viscosity of 8pa.S, mercapto group content of 6.50%) and 400g of toluene into a 1L clean three-necked flask, respectively, and remove the material by azeotropic dehydration. After the saturated water in the solution was cooled to below 80°C, under nitrogen protection and stirring, at the temperature of the reaction solution at 10-80°C, 1.0mol / L of n-butyllithium 206mL was continuously added dropwise within 20min to the reaction in the flask After 40 minutes of reaction, 0.6 mL of ethanol was inhaled with a syringe and injected into the reaction bottle to terminate the reaction for 20 minutes.

[0062] The second step is to add 18.5 g of epichlorohydrin to the reaction solution of the first step, stir the reaction at 50-80 ° C for 60 minutes, then add 20 mL of deionized water to the reaction solution and stir for 15 minutes, and then the water phase is removed statically. Final...

Embodiment 2

[0065] The relevant process conditions in Example 1 were kept unchanged.

[0066] The polysulfide rubber selected in the first step is JLY-1225 type (average molecular weight is 2500, viscosity 17pa.S, mercapto group mass content 2.62%) 100g, toluene 100g, n-butyllithium used is 87mL, the reaction time 30min, add 0.5mL of terminating agent ethanol.

[0067] 8.08 g of epichlorohydrin was added in the second step reaction, the reaction time was 120 min, after the reaction was completed, 30 mL of deionized water was used to stir for 15 min, the water phase was statically separated, and the solvent and other low-boiling organic impurities were removed by distillation under reduced pressure. . The viscosity of the amber viscous liquid measured by analysis is 18.5pa.S, and the epoxy value is 0.076mol / 100g.

Embodiment 3

[0069] The relevant process conditions in Example 1 were kept unchanged.

[0070] The polysulfide rubber selected in the first step is JLY-124 type (average molecular weight is 4000, viscosity 70pa.S, mercapto group mass content 1.64%) 100g, toluene 300g, n-butyllithium used is 54mL, the reaction time 25min, 0.4mL of terminating agent ethanol was added.

[0071] 4.8 g of epichlorohydrin was added in the second step reaction, the reaction time was 80 min, after the reaction was completed, 40 mL of deionized water was used to stir for 15 min, the water phase was statically separated, and the solvent and other low-boiling organic compounds were removed by distillation under reduced pressure. impurities. The viscosity of the amber viscous liquid measured by analysis is 72.1pa.S, and the epoxy value is 0.048mol / 100g.

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Abstract

The invention belongs to the technical field of polymer modification, and specifically discloses a preparation method of epoxy-terminated polysulfide rubber. The polysulfide rubber is reacted with an alkyl lithium reagent in advance, and the thiol groups in the polysulfide rubber are converted into sulfur-lithium bonds. , the sulfur-lithium polymer is obtained; then the sulfur-lithium polymer and the epoxy organochlorine raw material are subjected to an end-capping reaction to obtain. The invention also discloses a modified epoxy-terminated polysulfide rubber and the application of the product. In the preparation process of the epoxy-terminated polysulfide rubber of the present invention, the sulfur-lithium group formed by the reaction of highly active alkyl lithium with the thiol in the polysulfide rubber molecule is used to react with the epoxy organochlorine raw material, and the reaction belongs to Homogeneous reaction, fast reaction rate, no side reactions and so on. After the epoxy-terminated polysulfide rubber of the present invention is cross-linked with a small amount of amines, its tensile strength is not less than 3.0Mpa, its relative elongation is not less than 320%, its hardness (Shore A) is 65, and its glass transition temperature Tg is not high. At ‑16℃, the permanent deformation is not higher than 40%.

Description

technical field [0001] The invention relates to the field of epoxy-terminated polysulfide rubber, in particular to an epoxy-terminated polysulfide polymer, a preparation method and application thereof. Background technique [0002] Polysulfide rubber is a kind of synthetic rubber, which belongs to special rubber; it is a synthetic rubber obtained by polycondensation of dihaloalkane and polysulfide of alkali metal or alkaline earth metal. Industrial products include solid polysulfide rubber, liquid polysulfide rubber and polysulfide latex. Polysulfide rubber has excellent oil resistance and solvent resistance, but the strength is not high. Polysulfide rubber has good aging resistance, poor processing performance and odor. [0003] Zinc oxide, lead peroxide and manganese oxide for polysulfide rubber have excellent properties such as low temperature flexibility, solvent resistance and stress relaxation after vulcanization. They are mainly used in the manufacture of oil hoses, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/14C08G75/16C08L63/00C08L81/04C09J181/04C09K3/10
CPCC08G75/14C08G75/16C08L63/00C09J181/04C09K3/10C08L81/04Y02E60/10
Inventor 张建国刘篪姚谅蒋文英
Owner CHINA PETROLEUM & CHEM CORP
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