Preparing method for starch sulphate ammonium salt
A technology of ester ammonium salt and starch, which is applied in the field of starch sulfate ammonium salt and its preparation, can solve the problems of low substitution degree of sulfonic acid groups, high cost of sulfonating agent and solvent, serious degradation of starch molecules, etc. The effect of odor on human body toxicity, low raw material cost and equipment requirements, and convenient operation
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Embodiment 1
[0022] In the kneader, first put in sulfamic acid according to the molar ratio of starch sugar unit and sulfamic acid as 1:1.2, then put in urea according to the molar ratio of starch sugar unit and urea as 1:0.8, mix and heat to 150°C After it is completely melted, put in corn starch with a molar ratio of starch sugar unit of 1:1 and a purity of 87%. After constant temperature reaction until no water vapor is generated in the kettle, cool down to room temperature and use ammonia water to neutralize the residual acid in the reaction system to pH8. , add purity 95% ethanol to precipitate out, centrifuge at a centrifugal speed of 3500 rpm, and dry at 40°C to obtain a starch sulfate ammonium salt product with a sulfonic acid group substitution degree of 1.0.
Embodiment 2
[0024] Put sulfamic acid into the kneader according to the molar ratio of starch sugar unit and sulfamic acid as 1:1.0, then put urea into the kneader according to the molar ratio of starch sugar unit and urea as 1:1.2, mix and heat to 120°C, After it is completely melted, put in rice starch with a molar ratio of starch and sugar units of 1:1 and a purity of 90.2%. After constant temperature reaction until no water vapor is generated in the kettle, cool down to room temperature and use ammonia water to neutralize the residual acid in the reaction system to pH 10. Ethanol with a purity of 95% was added to precipitate a precipitate, centrifuged at a centrifugal speed of 5000 rpm, and dried at 50°C to obtain a starch sulfate ammonium product with a degree of substitution of sulfonic acid groups of 0.96.
Embodiment 3
[0026] Put sulfamic acid in the kneader according to the molar ratio of starch sugar unit to sulfamic acid as 1:1.5, then put urea into the kneader according to the molar ratio of starch sugar unit to urea as 1:1.0, mix and heat to 140°C, After it is completely melted, put in tapioca starch with a molar ratio of starch and sugar units of 1:1 and a purity of 96.5%. After constant temperature reaction until no water vapor is generated in the kettle, cool down to room temperature and use ammonia water to neutralize the residual acid in the reaction system to pH 10. Add 95% pure ethanol to precipitate out the precipitate, centrifuge at a centrifugal speed of 6000 rpm, and dry at 45°C to obtain a starch sulfate ammonium salt product with a degree of substitution of 0.98.
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