Method for preparing nanometer lamellar sodium carboxymethyl starch
A nano-scale technology of carboxymethyl starch sodium, which is applied in the field of preparation of carboxymethyl starch sodium, can solve the problems of easy gelatinization of starch, difficulty in penetrating into the interior of starch granules, and low utilization rate of etherifying agent, etc., to achieve Uniform particle size distribution, large specific surface, and smooth surface
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Embodiment 1
[0032] Add 16.0g of tapioca starch and 40g of absolute ethanol into a three-necked flask equipped with a thermometer and a stirrer, stir well to disperse the starch, heat to 40°C, add aqueous sodium hydroxide solution (7.0gNaOH, 30g of water) dropwise for alkalization , maintained at 40°C for 60 minutes to prepare a starch alkalization solution. After the starch was alkalized above, slowly add chloroacetic acid aqueous solution (7.0gClCH 2 COOH, 10g water), heated up to 45°C, reacted in a 400W (40kHz) ultrasonic wave for 20min, then maintained at 45°C for 80min, adjusted the pH value of the reaction solution to 7 with 6mol / L hydrochloric acid after the reaction, and filtered it with suction. The filter cake was washed with 70% ethanol aqueous solution until no chloride ion was detected in the filtrate, and the filter cake was dried at 60° C. to obtain 22.3 g of sodium carboxymethyl starch (CMS), the degree of substitution DS=1.31, and the scanning electron microscope (NovaNanoS...
Embodiment 2
[0034] Add 16.0g of tapioca starch and 50g of 60% ethanol aqueous solution into a three-necked flask equipped with a thermometer and agitator, stir well at 20°C to disperse the starch, add dropwise sodium hydroxide aqueous solution (3.0gNaOH, 30g of water) for alkalization , maintained at 20°C for 20 minutes to prepare a starch alkalization solution, after the starch was alkalized above, slowly add chloroacetic acid aqueous solution (5.0gClCH 2COOH, 10g water), heated up to 30°C, reacted in an ultrasonic wave with a power of 150W (40kHz) for 5min, then maintained at 30°C for 40min, adjusted the pH value of the reaction solution to 7 with 6mol / L hydrochloric acid after the reaction, and filtered it with suction. The filter cake was washed with 70% aqueous ethanol until no chloride ions were detected in the filtrate, and the filter cake was dried at 65°C to obtain 15.1 g of sodium carboxymethyl starch (CMS), with a degree of substitution DS=0.22, round particles, rough surface, ...
Embodiment 3
[0036] Add 16.0 g of tapioca starch and 90% ethanol aqueous solution (50 g of absolute ethanol) into a three-necked flask equipped with a thermometer and a stirrer, stir well to disperse the starch, heat to 40° C., add dropwise an aqueous sodium hydroxide solution (4.0 g NaOH, 25g water) to carry out alkalization reaction, maintain the temperature for 40min to prepare starch alkalization solution, after the starch is alkalized above, slowly add chloroacetic acid aqueous solution (8.0g ClCH 2 COOH, 10g water), heated up to 40°C, placed in ultrasonic waves (400W-40kHz, 10min), and then maintained at a reaction temperature of 40°C for 80min. After the reaction is completed, use 6mol / L hydrochloric acid to neutralize the pH of the reaction solution to 7. After suction filtration, wash with 95% aqueous ethanol until no chloride ions are detected in the filtrate, and dry the filter cake at 50°C to obtain carboxymethyl starch. Sodium (CMS) 22.2g, degree of substitution DS=1.28, flaky...
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