Temperature-sensitive starch derivative and preparation method thereof
A technology of starch derivatives and temperature sensitivity, which is applied in the field of temperature-sensitive starch derivatives and its preparation, achieving the effects of excellent performance, good biocompatibility and low toxicity
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Embodiment 1
[0060] In the first step, 3-ethoxy-2-hydroxypropyl starch is prepared. Add 4.6 grams of starch to a 100 ml three-necked flask, add 16 ml of water to disperse, stir and heat to 80°C. 1 gram of sodium hydroxide is dissolved in 4 grams of water. Drop into a three-necked flask and alkalize for 1 hour. Then, 2.5 g of ethoxy glycidyl ether was added dropwise and reacted for 5 hours. After the reaction is completed, dilute with 200 ml of water, neutralize with hydrochloric acid, wash the product with a 90% (w / w) acetone aqueous solution, wash it to be chlorine-free, dry under infrared light, and weigh. The product was Soxhlet extracted for 24 hours. The degree of substitution is determined to be DS=0.38.
[0061] The second step is to prepare 3-ethoxy-2-hydroxypropyl carboxymethyl starch. Add 8.75 g of chloroacetic acid, 3.7 g of solid sodium hydroxide, 30 ml of isopropanol to a 100 ml three-necked flask and stir for 30 minutes, then add the 3-ethoxy-2-hydroxypropyl starch prepared...
Embodiment 2
[0065] In the first step, 3-butoxy-2 hydroxypropyl starch is prepared. Add 4.6 starches to a 100 ml three-necked flask, add 16 ml of water to disperse, stir and heat to 80°C. 1 gram of sodium hydroxide is dissolved in 4 grams of water. Drop into a three-necked bottle and alkalize for 1 hour. Then, 8 g of butoxyglycidyl glycidyl ether was added dropwise. The reaction time is 5h. After the reaction, dilute with 200 ml of water, neutralize with hydrochloric acid to neutrality, wash the product with 90% (w / w) acetone aqueous solution, wash it to be free of chloride ions, dry under infrared light, and weigh. The product was Soxhlet extracted for 24h. The degree of substitution measured according to the test method in Example 1 is DS=1.1.
[0066] The second step is to prepare 3-butoxy-2-hydroxypropyl carboxymethyl starch. Add 3.4 g of chloroacetic acid, 1.8 g of solid sodium hydroxide and 30 ml of isopropanol to a 100 ml three-necked flask. After stirring for 30 minutes, add the...
Embodiment 3
[0070] In the first step, 3-butoxy-2 hydroxypropyl starch is prepared. Add 4.6 g of starch to a 100 ml three-necked flask, add 16 ml of water to disperse, stir and heat to 80°C. 1 gram of sodium hydroxide is dissolved in 4 grams of water. Drop into a three-necked flask and alkalize for 1 hour. Then, 1 g of butoxy glycidyl ether was added dropwise. The reaction time is 5 hours. After the reaction, dilute with 200 ml of water, neutralize with hydrochloric acid to neutrality, wash the product with 90% (w / w) acetone aqueous solution, wash it to be free of chloride ions, dry under infrared light, and weigh. The product was Soxhlet extracted for 24 hours. The measured degree of substitution is DS=0.15.
[0071] The second step is to prepare 3-butoxy-2-hydroxypropyl carboxymethyl starch. Add 17.5 g of chloroacetic acid, 7.4 g of solid sodium hydroxide, and 30 ml of isopropanol to a 100 ml three-necked flask. After stirring for 30 minutes, add the 3-butoxy-2-hydroxypropyl starch pr...
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