A kind of 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 15 g of butyl rubber (weight average molecular weight is 160000, degree of unsaturation 1%), cut into pieces and place in a four-necked flask, add 300 ml of cyclohexane to dissolve. When the colloidal particles were completely dissolved, slowly add 0.83g acetic acid, 0.37g Tween 20 and 0.37g Tween 80 (5% of the mass of the butyl rubber) into the four-necked flask, and directly add 6.17g hydrogen peroxide (mass) after stirring for 10 minutes. The fraction is 30%) and stirred, and the epoxidation reaction was started, and the reaction was carried out at 40 °C for 4 h. After the reaction, neutralize the acid and alkali with sodium hydroxide solution with a mass concentration of 1%, adjust the pH value of the glue solution to 8, wash the glue solution with distilled water, and then use ethanol to flocculate the gel solution. The prepared epoxybutyl rubber was detected by nuclear magnetic resonance, as shown in the attachedfigure 1 As shown, the degree of double bond e...
Embodiment 2
[0035] Weigh 15 g of butyl rubber (weight average molecular weight is 160000, degree of unsaturation 1%), cut into pieces and place in a four-necked flask, add 300 ml of cyclohexane to dissolve. When the rubber particles are completely dissolved, slowly add 0.83g acetic acid and 1.2g Tween 20 (8% of the mass of the butyl rubber) to the four-necked flask, and directly add 7.71g hydrogen peroxide (30% by mass) after stirring for 10 minutes. , the epoxidation reaction was started, and the reaction was carried out at 40 °C for 4 h. After the reaction, neutralize the acid and alkali with sodium hydroxide solution with a mass concentration of 1%, adjust the pH value of the glue solution to 8, wash the glue solution with distilled water, and then use boiling water to strip the glue solution. The prepared epoxy butyl rubber was detected by the method of nuclear magnetic resonance, and the results were as follows figure 2 shown, the degree of double bond epoxidation is 54.7%
Embodiment 3
[0037] Weigh 15g of butyl rubber (weight average molecular weight is 270000, degree of unsaturation 2.5%), cut into pieces and place in a four-necked flask, add 300ml of cyclohexane to dissolve. When 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 gum) were slowly added to the four-necked flask, and stirred for 10 minutes. Take out 5.13g of glue and 10.27g of hydrogen peroxide (mass fraction of 30%) to stir and emulsify (the mass ratio of glue and hydrogen peroxide is 1:2), after 30 minutes of emulsification, add the remaining glue to start the epoxidation reaction for 5h , the reaction temperature was 45 °C. After the reaction, neutralize the acid and alkali with sodium hydroxide solution with a mass concentration of 1%, adjust the pH value of the glue solution to 8, wash the glue solution with distilled water, and then use ethanol to flocculate the gel solution. The prepared epoxy butyl rubber was ...
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