A kind of rubber antioxidant, its composition and its preparation and application
A technology of rubber anti-aging agent and composition, which is applied in the field of rubber anti-aging agent to achieve the effects of easy implementation, improved use efficiency, and improved migration resistance
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Embodiment 1
[0100] The preparation of embodiment 1 antioxidant composition
[0101] Mix allyl glycidyl ether (13.70g) and n-dodecanethiol (20.24g) at a molar ratio of 1.2:1, add 0.51g benzoin dimethyl ether (DMPA), add 35g tetrahydrofuran, use 100W, 365nm UV light irradiation, turn on the magnetic stirring, react at room temperature for 30 minutes, stop the reaction, the product mixture is rotary evaporated at 120 °C to remove solvent tetrahydrofuran, photoinitiator DMPA and excess allyl glycidyl ether, and then in Dry in a vacuum oven at 100°C for five hours to obtain 30.65 g of an intermediate product, the structure of which is shown in formula (i).
[0102]
[0103] Mix the intermediate product (30.65g) represented by formula (i) with N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylenediamine (31.19g) in a molar ratio of 1:1.2 , add 0.80g salicylic acid, react in molten state at 150°C for 8 hours, dilute with chloroform, wash three times with saturated aqueous sodium bicarbonate solution, ...
Embodiment 2
[0110] The preparation of embodiment 2 antioxidant
[0111] Repeat the process of Example 1, the difference is that the aftertreatment of the target product is different: after evaporating and concentrating the organic phase, the organic phase is washed and rotary evaporated several times with petroleum ether to obtain the anti-aging agent shown in formula (ii).
[0112] The target product shown in the formula (ii) that embodiment 2 obtains carries out infrared characterization, and the result is as follows Figure 4 shown in Figure 4 It can be found that the -OH peak appeared at 3368, the C-O peak of ether at 1115 remained, and the C-O peak of epoxy at 913 disappeared, indicating that the epoxy group successfully opened the ring and underwent an addition reaction with the amino group.
[0113] The target product shown in the formula (ii) that embodiment 2 obtains is carried out mass spectrum characterization, and the result is as follows Figure 5 shown, from Figure 5 It...
Embodiment 3
[0115] The preparation of embodiment 3 antioxidant composition
[0116] Allyl glycidyl ether (13.70g) was mixed with p-cresyl thiophenol (12.42g) in a molar ratio of 1.2:1, 20g toluene was added, after 0.39g AIBN was dissolved in 20g toluene, the toluene solution of AIBN was Add it dropwise to the reaction vessel within half an hour, then react at 75°C for 6 hours, stop the reaction, spin the product mixture at 120°C to remove the solvent toluene, AIBN and excess reactants, and transfer it to a vacuum oven at 100°C Drying in middle temperature for ten hours gave 22.40 g of intermediate product, the structure of which was shown in formula (iii).
[0117]
[0118]The intermediate product (22.40g) shown in formula (iii) was mixed with N-isopropyl-N'-phenyl-p-phenylenediamine (23.40g) in a molar ratio of 1:1.1, and 0.59g of triethylamine was added, Add 50g of xylene, react at 130°C for 10 hours, wash three times with saturated aqueous sodium bicarbonate solution, and then wash...
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