A double-end functionalized high styrene rubber and its preparation method
A high styrene rubber, functionalized technology, applied in the field of double-end functionalized high styrene copolymer and its preparation, can solve the problems of low functionalization degree, difficult solvent purification, low equipment utilization rate, etc. Interaction, increase hardness and dynamic mechanical properties, reduce shrinkage effect
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Embodiment 1
[0032] Under the protection of anaerobic, anhydrous, and argon, add 700ml of hexane and 3mol of metal lithium wire into a 1000ml three-necked flask equipped with a condenser, dropping funnel, and magnetic stirrer, raise the temperature to 50°C, and add Add 1.36 mol of trimethoxy (4-chlorobutoxy) silane solution slowly (drop rate: 0.5 mol / L) into the three-necked flask, stir while adding, and use cold oil to lower the temperature, and control the reaction temperature at 50-60°C , the dropwise addition time is 1h, after the dropwise addition is complete, the constant temperature reaction is continued for 2h, the crude product is filtered under an inert atmosphere to obtain a functionalized initiator, and finally an organolithium initiator containing silicon ether is obtained for future use.
[0033] In a jacketed 15L stainless steel reactor, the system was replaced 3 times with argon gas. In the polymerization kettle, add cyclohexane 4315g, styrene 420g (accounting for 35% of mo...
Embodiment 2
[0037] Under the protection of anaerobic, anhydrous, and argon, add 700ml of hexane and 3mol of metal lithium wire into a 1000ml three-necked flask equipped with a condenser, dropping funnel, and magnetic stirrer, raise the temperature to 50°C, and add Triethoxy (4-chlorobutoxy) silane solution 1.36mol, slowly dropwise (dropping rate 0.2mol / L) into the three-necked flask, stirring while dropping and using cold oil to cool down, control the reaction temperature at 50-60 ℃, the dropwise addition time is 1h, after the dropwise addition is complete, continue the constant temperature reaction for 2h, and filter the crude product under an inert atmosphere to obtain a functionalized initiator, and finally an organolithium initiator containing silicon ether, which is ready for use.
[0038] In a jacketed 15L stainless steel reactor, the system was replaced 3 times with argon gas. Add 4444g of cyclohexane, 330g of styrene (accounting for 27.5% of the total amount of monomers), 300g of ...
Embodiment 3
[0042] The preparation of the functionalized catalyst was the same as in Example 1.
[0043]In a jacketed 15L stainless steel reactor, the system was replaced 3 times with argon gas. Add hexanaphthene 2044g in polymerization kettle, styrene 324g (accounting for 27% of monomer total amount), butadiene 396g (account for monomer total amount 33%), add 8.0mmol functionalized organolithium initiator, heat up to 60°C, polymerize for 50min, and then press the mixture of 2.16g THF, 3777g cyclohexane, 216g (18% of the total monomer) styrene, and 264g (22% of the total monomer) butadiene into the The polymerization kettle continued to react for 70 minutes. After the monomers were completely converted, the temperature was raised to 80° C., and 24.3 mmol of carbon dioxide end-capping agent was added twice to carry out the end-capping reaction. The reaction time was 80 minutes. After the reaction was completed, 10 g of antioxidant 1076 [3,5-di-tert-butyl-4-hydroxyphenylpropionate octadecy...
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