Preparation method of carboxymethyl chitosan quaternary ammonium salt in water phase by microwave irradiation
A technology of carboxymethyl chitosan and microwave radiation is applied in the field of preparation of carboxymethyl chitosan quaternary ammonium salt, which can solve the problems of difficult to control experimental conditions, long reaction time, cumbersome steps and the like, and achieves simplified preparation process, The effect of saving reaction time and improving product yield
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Embodiment 1
[0013] Example 1: 2 mL of 40 g / ml NaOH solution was added to 1 g of chitosan (the weight average molecular weight was 320,000, and the degree of deacetylation was 90%) and frozen at -15° C. After natural thawing, add 20mL 5g / ml NaOH solution and stir until the chitosan is evenly dispersed. According to chitosan: chloroacetic acid molar ratio is 1: 3 slowly drips chloroacetic acid solution (purity is greater than 97%), puts into the microwave radiation instrument after stirring evenly and carries out microwave radiation reaction for the first time, and its output power is 200W, radiation The time is 50 min and the temperature is 50°C. The carboxymethyl chitosan product is precipitated with acetone, and then the carboxymethyl chitosan product is dissolved in water to adjust the pH value to 14. According to chitosan and 2,3-epoxypropyltrimethylammonium chloride molar ratio is 1: 10, slowly drips 2,3-epoxypropyltrimethylammonium chloride solution (purity greater than 95%) ), sti...
Embodiment 2
[0014] Example 2: Add 2 mL of 50 g / ml NaOH solution to 1 g of chitosan (weight average molecular weight: 280,000, deacetylation degree: 95%) and freeze at -25°C. After natural thawing, add 10mL 20g / ml NaOH solution and stir until the chitosan is evenly dispersed. According to chitosan: chloroacetic acid molar ratio is 1: 5 slowly drips chloroacetic acid solution (purity is greater than 97%), puts into the microwave radiation instrument after stirring evenly and carries out microwave radiation reaction for the first time, and its output power is 600W, radiation The time is 30 minutes and the temperature is 90°C. The carboxymethyl chitosan product is precipitated with acetone, and then the carboxymethyl chitosan product is dissolved in water to adjust the pH value to 8. According to chitosan and 2,3-epoxypropyltrimethylammonium chloride molar ratio is 1: 12, slowly drips 2,3-epoxypropyltrimethylammonium chloride solution (purity greater than 95%) ), stirred evenly and placed i...
Embodiment 3
[0015] Example 3: 3 mL of 50 g / ml NaOH solution was added to 1 g of chitosan (weight average molecular weight: 220,000, deacetylation degree: 80%) and frozen at -18°C. After natural thawing, add 15mL 60g / ml NaOH solution and stir until the chitosan is evenly dispersed. According to chitosan: chloroacetic acid molar ratio is 1: 8 slowly drips chloroacetic acid solution (purity is greater than 97%), puts into the microwave radiation instrument after stirring evenly and carries out microwave radiation reaction for the first time, and its output power is 500W, radiation The time is 5 minutes and the temperature is 70°C. The carboxymethyl chitosan product is precipitated with acetone, and then the carboxymethyl chitosan product is dissolved in water to adjust the pH value to 9. According to chitosan and 2,3-epoxypropyltrimethylammonium chloride molar ratio is 1: 6, slowly drips 2,3-epoxypropyltrimethylammonium chloride solution (purity greater than 95%) ), stirred evenly and plac...
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