Protected catalytic composition and its preparation and use thereof for preparing polymers from ethylenically unsaturated monomers
A composition and polymer technology, applied in protected catalytic composition and its preparation, and in the application field of preparing polymers from ethylenically unsaturated monomers, which can solve the problems of difficult control of pre-polymerization
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Embodiment 1
[0141] Example 1 Preparation of a fully saturated protective substance by emulsion polymerization
[0142] The reactants and other components used in Examples 1.a-1.j can be found in Table A above. In this example, the emulsion polymerization was carried out in a 4 liter four necked round bottom flask equipped with a mechanical stirrer, temperature control, condenser, monomer and initiator feeds and nitrogen inlet. Deionized water (200 grams), anionic surfactant (18.8 grams) and Me-β-CD (59.2 grams) were added to the reaction flask at room temperature. These were heated to 85°C while purging with nitrogen and stirring. An emulsified monomer mix of deionized water, anionic surfactant, and monomer was prepared according to Table 1.A (all weights are in grams).
[0143] Table 1.A Composition of monomer mixtures used to prepare protective substances 1.a-1.j
[0144]
EMM a
h 2 o
superficial
sex agent
BA
EA
LA
Sty...
Embodiment 2
[0149] Example 2.A. Preparation of Fully Saturated Protective Substances by Solution Polymerization in Toluene Solvent
[0150] In this example, solution polymerization was carried out in a 1 liter four necked round bottom flask equipped with a mechanical stirrer, temperature control, condenser, monomer and initiator feeds and nitrogen inlet. Toluene (185 g) and BA (16.8 g) were added to the reaction flask at room temperature. These were heated to 65°C while purging with nitrogen and stirring. A solution of 0.24 grams of Lupersol 11 dissolved in 14 grams of toluene was added to the reaction flask at 65°C. A monomer mix containing 135 grams of BA and 15 grams of nDDM was added over 45 minutes. After the addition, the reaction mixture was held at 65°C for 15 minutes. These were heated to 80°C and a solution of 0.24 g of Lupersol 11 dissolved in 10 g of toluene was added. The reaction mixture was maintained at 80°C for 1 hour. The protective substance (1.d) was isolated by...
Embodiment 3
[0161] Embodiment 3. Preparation of organometallic catalyst components
[0162] Triphenylphosphine (390 mg, 1.50 mmol) and tetrachloro-1,4-benzoquinone (370 mg, 1.50 mmol), 10 mL of methanol and 50 mL of toluene were added to a 100 mL serum bottle under nitrogen. After stirring for 30 min (mechanical stirrer), this solution was added under nitrogen to another 100 mL serum vial containing bis(1,5-cyclooctadiene)nickel (45 mg, 165 micromol). The solution was stirred (mechanical stirrer) for 30 min, then the solvent was removed by evaporation (35°C, reduced pressure) until the total solution volume reached 40 mL.
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