A kind of preparation method of ionic rubber crosslinking agent
A cross-linking agent and ionic technology, applied in the field of cross-linked networks, can solve the problems of difficult recycling, environmental pollution, resource waste, etc., and achieve the effect of simple process, convenient recycling and biodegradation, and low cost
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[0016] A preparation method of an ionic rubber crosslinking agent, which adopts zinc methacrylate (ZDMA) and bis-[γ-(triethoxysilyl)propyl]tetrasulfide (Si-69) to prepare the ionic crosslinking agent , including the following steps:
[0017] 1) Mix 0.25-20 g ZDMA with 7.5-600 mL N-methyl-2-pyrrolidone (NMP), and dissolve uniformly with the aid of an ultrasonic cleaner to obtain a solution;
[0018] 2) Add 0.5-5 g formic acid, 0.25-20 g hydrogen peroxide with a concentration of 35% and 0.25-20 mL Si-69 to the solution obtained in step 1) respectively, and react at 90 °C for 12 h to obtain a reaction solution;
[0019] 3) The reaction solution obtained in step 2) was centrifuged at 3500 rpm, and the precipitate was repeatedly washed with 95% ethanol for 5 times, and then placed in an oven at 85°C for 12 hours to obtain an ionic crosslinking agent.
Embodiment 1
[0021] 1) Mix 8g ZDMA with 300mL N-methyl-2-pyrrolidone (NMP), and dissolve it uniformly with the aid of an ultrasonic cleaner;
[0022] 2) Add 1.97g formic acid, 14.48g hydrogen peroxide (35%) and 8mL Si-69 to the solution obtained in step 1) respectively, and react at 90 °C for 12 h;
[0023] 3) The reaction solution obtained in step 2) was centrifuged at 3500 rpm, and the lower layer of the precipitate was repeatedly washed with ethanol (95%) for 5 times, and then placed in an 85°C oven to dry for 12 hours to obtain an ionic crosslinking agent.
[0024] The mass of the ionic crosslinking agent prepared by Example 1 was 4.2 g, and the yield was 52.5%.
Embodiment 2
[0026] (1) Mix 10 g of ZDMA with 300 mL of N-methyl-2-pyrrolidone (NMP), and dissolve it uniformly with the aid of an ultrasonic cleaner;
[0027] (2) 1.97 g of formic acid, 14.48 g of hydrogen peroxide (35%) and 10 mL of Si-69 were added to the solution obtained in step (1) respectively, and the reaction was carried out at 90 °C for 12 h;
[0028] (3) The reaction solution obtained in step (2) was centrifuged at 3500 rpm, and the lower layer of the precipitate was repeatedly washed with ethanol (95%) for 5 times, and then placed in an oven at 85 °C for 12 h to obtain an ionic crosslinking agent.
[0029] The quality of the ionic crosslinking agent prepared by embodiment two is 5.2 g, and the productive rate is 52.0%
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