Construction method and application of a supramolecular hydrogel material
A supramolecular hydrogel and structural formula technology, applied in the field of new materials, can solve problems such as complex operating conditions, irreversibility, and undisclosed methods of constructing hybrid supramolecular hydrogel materials through electrostatic interactions
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Embodiment 1
[0096] 1. Preparation method
[0097] 1.1 Synthesis of glutamic acid-terminated polyethylene glycol
[0098] 1) 5g (0.5mmol) of polyethylene glycol (HO-PEG 227 -OH) and excess succinic anhydride in 250 mL of anhydrous dichloromethane, after 2 days of reaction at 45 ° C, the excess anhydride was removed by adding water and hydrolyzing it, followed by liquid separation and washing, and the organic layer was spin-dried to dry the solvent and vacuum-dried to obtain a Carboxylated polyethylene glycol (HOOC-PEG 227 -COOH);
[0099] 2) Take 3.0g of HOOC-PEG 227 -COOH, add 1.1 equivalents of N,N'-dicyclohexylcarbodiimide (0.133g), 1.05 equivalents of N-hydroxysuccinimide (0.071g), 0.01 equivalents of DMAP (0.72mg ), about 80 mL of anhydrous tetrahydrofuran, reacted in an ice-water bath for 5 minutes, and a certain amount of insoluble N, N'-dicycloethylurea (DCU) was produced. After reacting overnight, place in a refrigerator at 4° C. for about 1 hour, and filter to remove most of...
Embodiment 2
[0113] 1. Preparation method
[0114] 1.1 Synthesis of glutamic acid-terminated polyethylene glycol
[0115] 1) 3g (0.3mmol) of polyethylene glycol (HO-PEG 227 -OH) and excess succinic anhydride in 250 mL of anhydrous dichloromethane, after 3 days of reaction at 40 ° C, the excess anhydride was removed by adding water and hydrolyzing it, followed by liquid separation and washing, and the organic layer was spin-dried to dry the solvent and vacuum-dried to obtain a Carboxylated polyethylene glycol (HOOC-PEG 227 -COOH);
[0116] 2) Take 2.0g of HOOC-PEG 227 -COOH, add N,N'-dicyclohexylcarbodiimide (0.0824g), N-hydroxysuccinimide (0.0472g), DMAP (0.48mg), anhydrous tetrahydrofuran about 80mL, and react in an ice-water bath After 5 minutes, a certain amount of insoluble N,N'-dicycloethylurea (DCU) was produced. After reacting overnight, place in a refrigerator at 4° C. for about 1 hour, and filter to remove most of the DCU. After the filtrate was concentrated to two-thirds of...
Embodiment 3
[0130] 1. Preparation method
[0131] 1.1 Synthesis of glutamic acid-terminated polyethylene glycol
[0132] 1) 10g (1.0mmol) of polyethylene glycol (HO-PEG 227 -OH) and excess succinic anhydride in 250 mL of anhydrous dichloromethane, reacted at 50 °C for 1 day, and the excess anhydride was removed by adding water and hydrolyzing it, followed by liquid separation and washing, and the organic layer was spin-dried to dry the solvent and vacuum-dried to obtain a Carboxylated polyethylene glycol (HOOC-PEG 227 -COOH);
[0133] 2) Take 4.0g of HOOC-PEG 227 -COOH, N,N'-dicyclohexylcarbodiimide (0.177g), N-hydroxysuccinimide (0.0944g), DMAP (0.96mg), anhydrous tetrahydrofuran about 80mL, react in ice-water bath for 5min After that, a certain amount of insoluble N,N'-dicycloethylurea (DCU) was produced. After reacting overnight, place in a refrigerator at 4° C. for about 1 hour, and filter to remove most of the DCU. After the filtrate was concentrated to two-thirds of the origin...
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