Preparation method for quaternary phosphonium modified epoxidized natural rubber
A technology of natural rubber and epoxidation, which is applied in the field of preparation of epoxidized natural rubber, can solve problems such as the instability of phosphine-containing modified materials, and achieve the effects of mild conditions, simple and easy method, and good antibacterial effect
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Embodiment 1
[0028] Embodiment 1 Preparation steps of organic phosphine modified epoxidized natural rubber
[0029] (1) Dissolve epoxidized natural rubber in dichloromethane at a concentration of 50mg / ml. After it is completely dissolved, add bromoacetic acid dropwise under stirring. The molar ratio of bromoacetic acid to the initial epoxy group is 1.4:1. React The temperature was 30°C and the reaction time was 24 hours.
[0030] (2) Precipitate the above solution in excess methanol, and filter the product through dichloromethane-methanol secondary precipitation to obtain the ring-opened product of epoxidized natural rubber.
[0031] (3) Cut the above product into pieces and dissolve it in dichloromethane at a concentration of 20mg / ml, add triphenylphosphine, the molar ratio of triphenylphosphine to initial epoxy group is 1.1:1, and the reaction temperature is 25~ 30°C, the reaction time is 5 days.
[0032] (4) After the reaction, the above solution was concentrated, precipitated ...
Embodiment 2
[0033] Example 2 Fourier transform infrared spectrum, nuclear magnetic resonance spectrum and plasma emission spectrum test analysis data ( Figure 1~4 )
[0034] figure 1 with 2 Is the infrared spectrum of the ring-opening product, 3440cm -1 and 1736cm -1 The characteristic absorption peaks of hydroxyl and carbonyl appear at 868cm -1 The stretching vibration peak of the epoxy group decreases, indicating that the bromoacetic acid causes the ring-opening reaction of the epoxidized natural rubber. At the same time 1080cm -1 The stretching vibration peak of the furan ring appears at , which is caused by the side reaction of ring expansion during the ring opening process.
[0035] image 3 Infrared spectrum of the polymer grafted with quaternary phosphonium salt groups, 748cm -1 and 690cm -1 is the out-of-plane deformation vibration of the C-H bond on the benzene ring, indicating that triphenylphosphine has been successfully immobilized in epoxidized natural rubber.
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Embodiment 3
[0040] Embodiment 3 antibacterial experiment procedure and result
[0041] In a sterile environment, draw 50 μL of the frozen bacterial solution, add it to 2 mL of LB culture solution, and incubate overnight at 37°C, then take 100 μL of the above bacterial solution and add it to 50mL of LB culture solution, and shake it at 37°C for 4 hours. The concentration is about 10 7 -10 8 CFU, used as antibacterial test bacteria suspension. Cut the rubber sample into pieces as much as possible, put it into a 50mL Erlenmeyer flask filled with 9mL of normal saline after ultraviolet disinfection, then add 1mL of the test bacteria suspension, shake and cultivate in a shaker at 90r / min for 24h, and keep a constant temperature of 37°C. At the same time, a control group without samples and a blank control group were set up. Take 10min, and after 24h, 100μL of the bacterial solution was serially diluted, and the number of viable bacteria was calculated by the plate counting method.
[0042...
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