Preparation method of epoxidized butyl rubber
A technology for epoxidizing butyl and butyl rubber, which is applied in the chemical industry, can solve the problems of inability to achieve high epoxidation degree and high cost, and achieve the effects of improving dispersion, broadening channels, and improving mechanical properties
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Embodiment 1
[0033] Weigh 15g of butyl rubber (weight average molecular weight: 160,000, degree of unsaturation: 1%), cut into pieces and place in a four-neck flask, add 300ml of cyclohexane to dissolve. Slowly add 0.83g acetic acid and 0.37g Tween 20 and 0.37g Tween 80 (5% of the butyl gum quality) in the four-necked flask after the micelle dissolves completely, after stirring for 10 minutes, directly add 6.17g hydrogen peroxide (mass. Fraction is 30%) stirring, start the epoxidation reaction, react at 40 ℃ for 4h. After the reaction is finished, acid-base neutralization is carried out with a sodium hydroxide solution with a mass concentration of 1%, the pH value of the glue solution is adjusted to 8, the glue solution is washed with distilled water, and then ethanol is used to flocculate the gel solution. The epoxy butyl rubber prepared by nuclear magnetic resonance detection, as attachedfigure 1 As shown, the degree of double bond epoxidation is 22.6%.
Embodiment 2
[0035] Weigh 15g of butyl rubber (weight average molecular weight: 160,000, degree of unsaturation: 1%), cut into pieces and place in a four-neck flask, add 300ml of cyclohexane to dissolve. Slowly add 0.83g acetic acid and 1.2g Tween 20 (8% of the butyl gum mass) in the four-necked flask after the colloidal particles are completely dissolved, after stirring for 10 minutes, directly add 7.71g hydrogen peroxide (mass fraction is 30%) and stir , Start the epoxidation reaction, and react at 40°C for 4h. After the reaction is finished, use a sodium hydroxide solution with a mass concentration of 1% for acid-base neutralization, adjust the pH value of the glue to 8, wash the glue with distilled water, and then use boiling water to strip the glue. The prepared epoxy butyl rubber is detected by the method of nuclear magnetic resonance, and the results are as attached figure 2 As shown, the degree of double bond epoxidation is 54.7%
Embodiment 3
[0037] Weigh 15g of butyl rubber (weight average molecular weight: 270,000, degree of unsaturation: 2.5%), cut into pieces and place in a four-neck flask, add 300ml of cyclohexane to dissolve. After the colloidal particles were completely dissolved, 1.04 g of formic acid and 0.45 g of Tween 80 (3% of the mass of the butyl rubber) were slowly added into the four-necked flask, and stirred for 10 minutes. Take out 5.13g of glue and 10.27g of hydrogen peroxide (mass fraction is 30%) and stir emulsification (the mass ratio of glue to hydrogen peroxide is 1:2). After emulsification for 30 minutes, add the remaining glue to start the epoxidation reaction and react for 5h , and the reaction temperature was 45°C. After the reaction is finished, acid-base neutralization is carried out with a sodium hydroxide solution with a mass concentration of 1%, the pH value of the glue solution is adjusted to 8, the glue solution is washed with distilled water, and then ethanol is used to flocculat...
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