Supermolecule material and self repairing hydrogel
A supramolecular and hydrogel technology, applied in the field of supramolecular chemistry, can solve problems such as inability to complete self-healing
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[0089] Example 1
[0090] The embodiment of the present invention provides the preparation method of formula six and formula seven, and the specific steps are as follows:
[0091] The preparation method of formula six is as follows: p-toluenesulfonyl imidazole (8.9 g, 40 mmol) and β cyclodextrin (β-CD, 35 g, 30.84 mmol) are added to 250 ml of distilled water and stirred to form a white suspension. After reacting for 4 hours under stirring at room temperature, 50 ml of sodium hydroxide solution with a mass fraction of 20% was added, and stirring was continued for 30 minutes, the reaction liquid changed from milky white to light yellow. Filter to remove insoluble materials, transfer the filtrate to a 500ml beaker, and add 1.5mol / L hydrochloric acid to adjust the pH to neutral. Place the beaker in a low temperature environment of 4°C to cool and crystallize for 12 hours. Filter, wash with deionized water and wash the crude product with acetone. Then heated and recrystallized twic...
Example Embodiment
[0093] Example 2
[0094] The characterization test of Formula 6 and Formula 7 of Example 1, the results are as follows:
[0095] Formula six:
[0096] 1 HNMR(400MHz,DMSO-d 6 ): 5.60~5.89(m,14H), 4.75~4.81(m,7H), 4.15~4.62(m,6H), 3.45~3.72(m,28H), 3.15~3.47(m,14H), 2.41(s ,3H),2.90-3.04(m,2H),2.69-2.79(m,1H).FT-IR(KBr,cm -1 ):3354,2929,2131,1705,1638,1414,1366,1233,1156,1028,946,859,756,706,580.ESI-MS(m / z):calc ulated,1171.4for C 45 H 73 O 34 N,found 1172.5for[M+H] + .
[0097] Formula seven:
[0098] 1 HNMR(400MHz, CDCl 3 -d): 4.64(2H), 2.4(1H), 2.0(3H), 1.9(6H), 1.7(6H).FT-IR(KBr,cm -1 ): 3308, 2907, 2853, 2129, 1731, 1453, 1365, 1345, 1323, 1269, 1225, 1183, 1157, 1103, 1073,997.
Example Embodiment
[0099] Example 3
[0100] The embodiment of the present invention provides a preparation method of Formula 1, and the specific steps are as follows:
[0101] Formula One (R 1 for The preparation method of) is as follows: first, dipentaerythritol-based hexabromo ATRP initiator is prepared by esterification reaction from dipentaerythritol and 2-bromoisobutyryl bromide. The hexabromo initiator (0.0667g, 0.058mmol), NIPAM (4g, 35mmol), Me 6 TREN (0.080g, 0.35mmol) and 10mL solvent (V DMF :V water =80:20) Add to an anhydrous and oxygen-free bottle to fully dissolve. Vacuum-charge N 2 Three times in N 2 Quickly add CuBr (0.0504g, 0.35mmol) under protection, vacuum-fill N 2 three times. In N 2 Continue to stir and react for 2h under protection. After the reaction is completed, add 15ml of THF to dilute, and place it in the air and stir for 2h, then pass through a silica gel column to remove the cuprous bromide. Spin off the excess solvent, add the product to ice ether for precipitat...
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