Ethylene-propylene-diene monomer rubber graft copolymer and halogen-free flame-retardant ethylene-propylene-diene monomer rubber material and preparation method thereof
A technology of EPDM rubber and graft copolymer, which is applied in the field of preparing halogen-free flame-retardant EPDM materials and halogen-free flame-retardant EPDM materials. Reduced elongation at break and other issues to achieve good mechanical properties
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preparation example 1
[0096] Under the protection of nitrogen, add 0.76g of iodine, 0.85g of the compound represented by formula (2-2) and 20mL of dichloromethane into a 100mL three-necked flask, stir at 25°C for 0.5 hours, and dilute the obtained mixture with aluminum oxide Separation was carried out by column chromatography (the developing solvent was dichloromethane), and the obtained eluate was concentrated and washed with cyclohexane to obtain 1.31 g of a catalyst as a yellow solid. The obtained catalyst was subjected to H NMR spectroscopy ( 1 H-NMR) and carbon nuclear magnetic resonance ( 13 C-NMR) and X-ray single crystal diffraction analysis, confirmed that the obtained catalyst has a structure shown in formula (2-1).
[0097] 1 H-NMR(400MHz,DMSO)δ(ppm):1.35-2.06(m,33H),1.81(s,18H),2.62(m,4H),6.11(d,1H),7.38-7.50(m,5H ),7.59-7.67(m,3H).
[0098] 13 C-NMR (100MHz, DMSO) δ (ppm): 24.8, 25.5, 26.2, 26.3, 26.4, 26.6, 31.9, 32.1, 129.1, 129.2, 129.3, 129.5, 130.7, 134.2, 134.3, 193.0.
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Embodiment 1
[0101] Example 1: This example is used to illustrate the method for preparing EPDM graft copolymer provided by the present invention and the method for preparing halogen-free flame-retardant EPDM material
[0102] Weigh 0.1 g of the catalyst with the structure represented by formula (2-1), and dissolve it in 12 mL of xylene solution to obtain catalyst solution C1, which is set aside.
[0103] 5g EPDM rubber, 0.7g flame retardant monomer shown in formula (1) in 2 Under protection, dissolve in 70mL xylene solution until completely dissolved; then at 120°C, add 2mL catalyst solution C1 first, react for 10min, divide the remaining 10mL catalyst solution C1 into 5 parts, and add one part every 10min The method is added to the reaction system, and after the last part of catalyst solution C1 is added to the reaction system for 10 minutes, the reaction is stopped, and the total reaction time is 60 minutes. After the reaction was completed, the reaction solution was filtered with a ni...
Embodiment 2
[0107] This example was carried out by a method similar to that of Example 1, except that in this example, 12 mL of catalyst solution C1 was added to the reaction system at one time at 120° C., and reacted for 60 minutes. All the other are the same as in Example 1.
[0108] In this example, the halogen-free flame-retardant EPDM material A2 was obtained.
[0109]The relevant reaction conditions of this example are specifically listed in Table 1. The flame retardancy and mechanical properties of the halogen-free flame-retardant EPDM material A2 were analyzed and measured, and the results are shown in Table 2.
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