Liquid rubber and preparation method thereof
A liquid rubber and olefin technology, applied in the field of liquid rubber and its preparation, can solve the problems of substandard yellowness index, complicated treatment process and increased production cost, etc.
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[0012] The invention provides a method for preparing liquid rubber, which comprises the following steps: (1) polymerizing olefins under anionic polymerization conditions in the presence of an organolithium compound and a non-polar organic solvent; the organolithium compound and the The mol ratio of said olefin is 1: 70-1850; (2) the solution that step (1) polymerization obtains is mixed with water and / or C simultaneously or successively 1 -C 6 Alcohol and gas containing 10-100% by volume of carbon dioxide are contacted, and then the contacted product is heated and / or vacuum-dried in the presence of an anti-aging agent and under stirring conditions, relative to 1 mole of the step (1) The organolithium compound, the water and / or C 1 -C 6 The consumption of the alcohol is 0.5-1.5 moles, and the consumption of the carbon dioxide is 0.5-2 moles. In a preferred situation, relative to 1 mole of the organolithium compound in step (1), the water and / or C 1 -C 6 The amount of alcoh...
Embodiment 1
[0026] (1) In a 5L polymerization reactor (jacketed) after replacing the internal gas with high-purity nitrogen, add 200g of isoprene (purified by vacuum distillation) and 1800g of cyclohexane and mix evenly to obtain a solution, and heat it under stirring The solution was brought to 50° C., and 45 mL of n-butyllithium (0.1 mol / L, the solvent was cyclohexane) was added to the solution, and then the temperature of the solution was controlled at 50-70° C. for 120 minutes.
[0027] (2) Add 0.08mL of deionized water to the solution after the polymerization reaction under stirring, and simultaneously feed carbon dioxide (purity greater than 99.9% by weight) into the solution after the polymerization reaction at a flow rate of 10mL / min for 10 minutes, continue Stir for 5 minutes, then add 1 g of 2,6-di-tert-butyl-p-cresol. The vacuum degree in the reaction kettle was set at -100kPa, and the above solution was heated to 80° C. under stirring and kept for 4 hours to obtain a colorless...
Embodiment 2
[0038] (1) Carry out polymerization reaction according to the method for embodiment 1 step (1).
[0039] (2) Prepare liquid polyisoprene rubber according to the method of step (2) of Example 1, the difference is that 0.08mL of deionized water is first added, and then passed into the solution after the polymerization reaction at a flow rate of 10mL / min Carbon dioxide (purity greater than 99.9% by weight) for 5.5 minutes and continued stirring for 10 minutes. After drying, a colorless and transparent liquid polyisoprene rubber was obtained, and the content of the 1,4-structure in the liquid polyisoprene rubber was determined to be 94.5%. Take an appropriate amount of the above-mentioned liquid polyisoprene rubber and place it in an oven at 80° C. for 4 hours, and the appearance of the liquid polyisoprene rubber is still colorless and transparent.
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