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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Embodiment 1
[0090] The embodiment of the present invention provides the preparation method of formula 6 and formula 7, and the specific steps are as follows:
[0091] The preparation method of formula 6 is as follows: add p-toluenesulfonyl imidazole (8.9g, 40mmol) and β-cyclodextrin (β-CD, 35g, 30.84mmol) into 250ml of distilled water and stir 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 the stirring was continued for 30 min, and the reaction liquid changed from milky white to light yellow. Remove the insoluble matter by filtration, transfer the filtrate to a 500ml beaker, and add 1.5mol / L hydrochloric acid to adjust the pH to neutral. Place the beaker at 4°C for cooling and crystallization for 12 hours. Filter and wash the crude product with deionized water followed by acetone. Heated and recrystallized twice with deionized water, dried in vacuum for 48 hours, and...
Embodiment 2
[0094] The characterization detection carried out to formula six and formula seven of embodiment 1, the result is 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):calculated,1171.4for C 45 h 73 o 34 N, found 1172.5 for [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.
Embodiment 3
[0100] The embodiment of the present invention provides the preparation method of Formula 1, and the specific steps are as follows:
[0101] Formula 1 (R 1 for ) preparation method is as follows: first by dipentaerythritol and 2-bromoisobutyryl bromide by esterification preparation dipentaerythritol base hexabromo ATRP initiator, this hexabromo initiator (0.0667g, 0.058mmol), NIPAM (4g, 35mmol), Me 6 TREN (0.080g, 0.35mmol) and 10mL solvent (V DMF :V 水 =80:20) into an anhydrous and oxygen-free bottle to fully dissolve. Vacuum-fill N 2 three times at N 2 Quickly add CuBr (0.0504g, 0.35mmol) under protection, vacuum-fill with N 2 three times. in N 2 Continue to stir the reaction for 2 h under protection, add 15 ml of THF to dilute after the reaction, and stir in air for 2 h, pass through a silica gel column to remove cuprous bromide. Spin off the excess solvent, add the product to glacial ether to precipitate, repeat 2-3 times to fully remove unpolymerized monomers. ...
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