Modified hydrophilic polyrotaxane and cross-linked polyrotaxane
A hydrophilic polyrotaxane technology, applied in the field of hydrophilic modified polyrotaxane, can solve the problems of low mechanical strength and uneven structure
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Embodiment 1
[0132] (1) Preparation of PEG-carboxylic acid by TEMPO oxidation of PEG
[0133] 10 g of polyethylene glycol (PEG) (molecular weight: 5000), 100 mg of TEMPO (2,2,6,6-tetramethyl-1-piperidinyl-oxyl radical) and 1 g of sodium bromide were dissolved in 100 ml of water. A commercially available sodium hypochlorite aqueous solution (available chlorine concentration: 5%) was added in an amount of 5 ml, and stirred at room temperature for 10 minutes. To decompose excess sodium hypochlorite, ethanol in the range of up to 5 ml was added to terminate the reaction.
[0134] Extraction with 50 ml of dichloromethane was repeated three times, thereby extracting components other than inorganic salts. Thereafter dichloromethane was distilled off from the extracted fraction using an evaporator. Then, the fractions were dissolved in hot ethanol and then allowed to stand overnight in a freezer (-4°C) to extract only PEG-carboxylic acid, which was then recovered and dried.
[0135] (2) Prepara...
Embodiment 2
[0146] (1) Preparation of PEG-carboxylic acid by TEMPO oxidation of PEG
[0147] 10 g of polyethylene glycol (PEG) (molecular weight: 5000), 100 mg of TEMPO (2,2,6,6-tetramethyl-1-piperidinyl-oxyl radical) and 1 g of sodium bromide were dissolved in 100 ml of water. A commercially available sodium hypochlorite aqueous solution (available chlorine concentration: 5%) was added in an amount of 5 ml, and stirred at room temperature for 10 minutes. To decompose excess sodium hypochlorite, ethanol in the range of up to 5 ml was added to terminate the reaction.
[0148] Extraction with 50 ml of dichloromethane was repeated three times, thereby extracting components other than inorganic salts. Thereafter dichloromethane was distilled off from the extracted fraction using an evaporator. Then, the fractions were dissolved in hot ethanol and then allowed to stand overnight in a freezer (-4°C) to extract only PEG-carboxylic acid, which was then recovered and dried.
[0149] (2) Prepara...
Embodiment 3
[0160] (1) Preparation of PEG-carboxylic acid by TEMPO oxidation of PEG
[0161] 10 g of polyethylene glycol (PEG) (molecular weight: 100,000), 100 mg of TEMPO (2,2,6,6-tetramethyl-1-piperidinyl-oxyl radical) and 1 g of sodium bromide were dissolved in 100 ml of water. A commercially available sodium hypochlorite aqueous solution (available chlorine concentration: 5%) was added in an amount of 5 ml, and stirred at room temperature for 10 minutes. To decompose excess sodium hypochlorite, ethanol in the range of up to 5 ml was added to terminate the reaction.
[0162] Extraction with 50 ml of dichloromethane was repeated three times, thereby extracting components other than inorganic salts. Thereafter dichloromethane was distilled off from the extracted fraction using an evaporator. Then, the fractions were dissolved in hot ethanol and then allowed to stand overnight in a freezer (-4°C) to extract only PEG-carboxylic acid, which was then recovered and dried.
[0163] (2) Prep...
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