A chitin-based macromolecular chain transfer agent and its preparation method and application
A macromolecular chain and chitin technology, applied in the field of chitin macromolecular chain transfer agent, can solve the problem of not designing a macromolecular chain transfer agent
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Embodiment 1
[0056] The preparation of the macromolecule initiator 1 of embodiment 1 chitin
[0057] Mix 4g of chitin and 200g of ionic liquid (1-allyl-3-methylimidazolium bromide) and dissolve at 100°C for 12 hours under vacuum; add 180g of 2-bromopropane dropwise in an ice-water bath Acyl bromide, after the dropwise addition, react at room temperature for 48 hours. After the reaction is completed, the product is precipitated in water to obtain a yellow powder, which is washed several times with water and filtered with suction; the obtained yellow powder is vacuum-dried at 60°C for 24 hours to obtain The chitin initiator 1, the structure is as follows:
[0058]
[0059] in,
[0060] The resulting chitin macroinitiator 1 had a degree of substitution of 1.85 and a weight of 6.89 g. The proton nuclear magnetic spectrum figure of described chitin macromolecular initiator 1 is as figure 1 As shown, the infrared spectrum is shown in Figure 9 As shown, the thermogravimetric analysis sp...
Embodiment 2
[0061] The preparation of embodiment 2 chitin macromolecular initiator 2:
[0062] The preparation method of the present embodiment is the same as that of Example 1, except that the consumption of 2-bromopropionyl bromide is adjusted (promoting 220g), and the reaction time is increased to 72 hours simultaneously, so that the degree of substitution of the chitin macroinitiator 2 obtained It is 1.9 and the weight is 7.02g. The proton nuclear magnetic spectrum figure of described chitin macromolecular initiator 2 is as figure 2 shown.
[0063] The structure of chitin macroinitiator 2 is shown below:
[0064]
[0065] in,
Embodiment 3
[0066] The preparation of embodiment 3 chitin macromolecular chain transfer agent 1:
[0067] 4g chitin macroinitiator 1 was dissolved with 80ml dimethyl sulfoxide solvent. At the same time, 510 mg of ethanethiol and 830 mg of triethylamine were dissolved in 20 ml of dimethyl sulfoxide, mixed and stirred for 10 minutes, and then 1.874 g of carbon disulfide was added into the mixed solution. After the drug is completely dissolved, mix the two solutions. The mixed solution was reacted at 40° C. for 24 hours to obtain 3.42 g of ethyl chitin macromolecular chain transfer agent.
[0068] The H NMR spectrum of the chitin macromolecular chain transfer agent 1 is as follows image 3 As shown, the infrared spectrum is shown in Figure 10 As shown, the thermogravimetric analysis spectrum is as Figure 12 shown.
[0069] From 7.91ppm, it can be seen that the peak of the amide group is still there, and at the same time, from 1.29ppm, it can be seen that a new methyl peak has appeared...
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