Supramolecular material, temperature-sensitive hydrogel and preparation method thereof
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A temperature-sensitive hydrogel and supramolecular technology, applied in the field of supramolecular chemistry, can solve problems such as inability to complete self-healing
Active Publication Date: 2019-03-08
GUANGDONG UNIV OF TECH
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For larger cracks, when the two sides of the self-healing material section do not touch, it is often necessary to manually fit the two ends of the section together, otherwise the self-healing cannot be completed
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Embodiment 1
[0093] The embodiment of the present invention provides the preparation method of formula 6 and formula 7, and the specific steps are as follows:
[0094] 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 sodiumhydroxide 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
[0097] The characterization detection carried out to formula six and formula seven of embodiment 1, the result is as follows:
[0098] Formula six:
[0099] 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,1171.4forC 45 h 73 o 34 N, found 1172.5 for [M+H] + .
[0103] The embodiment of the present invention provides the preparation method of Formula 1, and the specific steps are as follows:
[0104] Formula 1 (L1 is R 1 for ) is prepared as follows: the two-way ATRP initiator prepared by the reaction of ethylene glycol and 2-bromoisobutyryl bromide, the two-way ATRP initiator (0.127g, 0.35mmol), NIPAM (8g, 70mmol), Me 6 TREN (0.161g, 0.70mmol) and 20mL solvent (V DMF :V 水 =80:20) into anhydrous and oxygen-free bottles respectively. Under stirring, vacuumize-fill with nitrogen three times, under the protection of nitrogen, quickly add CuBr (0.1 g, 0.70 mmol), then vacuumize-fill with nitrogen three times, and react at room temperature for 2 h under the protection of nitrogen. After the reaction was completed, 15 ml of tetrahydrofuran was added for dilution and exposed to air to terminate the reaction. Pass through a silica gel column to remove cuprous bromide. Rotary evaporation, the crude product was added to a large amount ...
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Abstract
The invention belongs to the technical field of supramolecular chemistry, and particularly relates to a supramolecular material, a temperature-sensitive hydrogel and a preparation method thereof. Thesupramolecular material comprises a first construction unit, a second construction unit and a third construction unit, wherein the first construction unit is provided with a structure as shown in theformula I; the second construction unit is provided with a structure as shown in the formula II; the third construction unit is provided with a structure as shown in the formula III or / and formula IV;and the first construction unit, the second construction unit and the third construction unit are self-assembled and connected to form the supramolecular material based on adamantane-cyclodextrin subjective and objective bodies. The invention further provides a hydrogen which is prepared through the following steps of mixing the first construction unit, the second construction unit, the third construction unit and water; performing self-assembly through the adamantane-cyclodextrin subjective and objective bodies of the first construction unit, the second construction unit and the third construction unit so as to form the hydrogel. The hydrogel provided by the invention solves the technical problems that an existing hydrogel is disordered in structure and incapable of being adjusted and controlled, and requires manual fitting for macroscopic big-crack self-repairing.
Description
technical field [0001] The invention belongs to the technical field of supramolecular chemistry, and in particular relates to a supramolecular material, a temperature-sensitive hydrogel and a preparation method thereof. Background technique [0002] Self-healing is the most basic property of living organisms, such as skin and bone can automatically heal itself after injury. Hydrogels are usually soft and elastic, with a high water content. These properties make hydrogels very similar to biological tissue structures. Therefore, through reasonable design, hydrogel materials can also achieve self-healing functions similar to biological organisms. . Hydrogels with self-healing function can automatically repair the regional damage of materials caused by extreme external conditions (such as large deformation or external force damage), and restore the damaged gel to its shape and function, thereby prolonging the life of the gel material. Working life and service stability, optimi...
Claims
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