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Improved preparation method of epoxy trans isoprene rubber

A technology of trans-isoprene rubber and epoxidation, applied in the field of improved epoxidized trans-isoprene rubber preparation, can solve the problems of instability, difficult epoxidation reaction, uneven distribution of epoxy groups, and the like, To achieve the effect of improving adhesion

Inactive Publication Date: 2014-07-09
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this aqueous phase suspension method overcomes the shortcoming of above-mentioned latex method and solution method epoxidation modification, as the recovery and aftertreatment process that adds organic solvent to bring is complicated, but because aqueous phase suspension method and powdery trans-1, The characteristics of 4-polyisoprene, the distribution of epoxy groups in the prepared epoxidized trans-1,4-polyisoprene is uneven, often forming a layer on the surface of the powdered polymer Epoxy compounds with extremely high epoxidation degree and dense structure make the continuous epoxidation reaction relatively difficult. At the same time, the uneven distribution of epoxy groups will also lead to inhomogeneous and uneven performance during processing and use. Stablize

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Wash and dry a 1000mL three-necked flask, add 150g of toluene solution of trans isoprene rubber, wherein the content of trans isoprene rubber is 30g, start stirring, add 2g of sodium dodecylbenzene sulfonate to dissolve it completely, and then Slowly add 200ml of distilled water, and stir for 30 to 90 minutes at a speed of 800 to 2000 rpm to disperse the copolymerized rubber into an emulsion state; according to organic acid / trans isoprene rubber double bond = 0.8 (molar ratio), hydrogen peroxide / Slowly add acetic acid and hydrogen peroxide to the system at a ratio of organic acid=1.2:1, control the system temperature at 50 degrees, and react for 8 hours. 5 g of methanol was added to perform demulsification. Then it was suction filtered and washed 3 times with distilled water, and weighed after drying. Gained epoxidized trans isoprene rubber was 35g, and its epoxy group content was 71.8% calculated by nuclear magnetic method.

Embodiment 2

[0024] Wash the 50L reactor, add 20000mL of toluene and 2000g of trans isoprene rubber, raise the temperature to 40 degrees and start stirring to dissolve the polymer, according to the organic acid / trans isoprene rubber double bond = 0.4 (molar ratio) 1. Slowly add acetic acid and hydrogen peroxide to the system at a ratio of hydrogen peroxide / organic acid=1.15:1, control the temperature of the system at 40 degrees, and react for 6 hours. After stopping the reaction, the whole system was poured into boiling water, and the solvent was recovered. Then neutralize the polymer slurry with dilute sodium bicarbonate solution to neutrality, filter with suction and wash with distilled water for 3 times, weigh after drying. Gained epoxidized trans isoprene rubber was 2360g, and its epoxy group content was 38.7% calculated by nuclear magnetic method. Performance tests show that the cord pull-out force of epoxidized trans isoprene rubber is 4.87 times higher than that of non-epoxidized t...

Embodiment 3

[0026]Wash and dry a 5000mL three-neck flask, add 2000mL of toluene and 200g of trans isoprene rubber, heat up to 40 degrees and start stirring to dissolve the polymer, according to organic acid / trans isoprene rubber double bond = 0.5 (mol Ratio), hydrogen peroxide / organic acid=1.15:1, slowly add acetic acid and hydrogen peroxide to the system, control the system temperature to 40 degrees, and react for 6 hours. After stopping the reaction, the whole system was poured into boiling water, and the solvent was recovered. Then neutralize the polymer slurry with a dilute sodium hydroxide solution to neutrality, filter it with suction and wash it with distilled water for 3 times, and weigh it after drying. Gained epoxidized trans isoprene rubber was 228g, and its epoxy group content was calculated to be 48.3% by nuclear magnetic method.

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PUM

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Abstract

The invention provides an improved preparation method of epoxy trans isoprene rubber, and relates to the field of polymer materials. A first preparation method comprises the following steps: dissolving trans isoprene rubber in a solvent, slowly adding an organic acid and hydrogen peroxide under a stirring and / or ultrasonic action, reacting at a temperature of 0-80 DEG C for 0.1-12 hours, adding sodium carbonate to regulate the pH of the system to 7 after the reaction, removing a sweller and water by use of a vaporizing extract process, repeatedly eluting, pelleting and drying, and epoxy trans isoprene rubber with epoxy groups uniformly distributed in a polymer is obtained by the preparation method; a second preparation method comprises the following steps: partially dissolving the trans isoprene rubber in the sweller, wherein the rest steps are the same as those in the first method; a third preparation method comprises the following steps: prefabricating the trans isoprene rubber to emulsion, wherein the rest steps are the same as those in the first method. The epoxy groups are introduced to increase the wet skid resistance and air tightness of the trans isoprene rubber and the binding power of polar compounds, and the epoxy trans isoprene rubber can be applied on such occasions as a conveyor belt, a tire and a damping material.

Description

technical field [0001] The invention belongs to the field of polydiene rubber materials, and particularly relates to an improved preparation method of epoxidized trans isoprene rubber. The epoxidized trans isoprene rubber prepared by the method has more uniform distribution of epoxy groups and has It is beneficial to improve the adhesion, wet skid resistance and air tightness between non-polar trans-isoprene rubber and polar substances, and can be used in conveyor belts, rubber for tires and shock-absorbing materials. Background technique [0002] Trans-isoprene rubber is a natural or synthetic rubber whose structural unit is trans-1,4-isoprene. Trans isoprene rubber has excellent wear resistance, dynamic fatigue resistance, high modulus stress and partial crystallization, and can be used in rubber tires, rubber shoes, medical splints, shape memory materials, conveyor belts, shock absorbers, etc. It is used in occasions where high fatigue performance is required. However, ...

Claims

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Application Information

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IPC IPC(8): C08F36/08C08F8/08
Inventor 姚薇邵华锋刘晨光姜秀波
Owner QINGDAO UNIV OF SCI & TECH
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