Method for preparing matrine/carboxymethyl chitosan/phosphonic chitosan pesticide nanoparticle aqueous dispersion preparation
A technology of phosphorylated chitosan and carboxymethyl chitosan, applied in the fields of botanical equipment and methods, agriculture, biocide, etc., can solve the problems of easy decomposition of active ingredients, complex preparation ingredients, unstable to light, etc. To achieve the effect of easy preparation, favorable adhesion and penetration, and avoiding the use of organic solvents and other additives
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Embodiment 1
[0023] (1) Preparation of phosphorylated chitosan: The viscosity average molecular weight of 5g is 8.5×10 4 , The chitosan with a degree of deacetylation of 95% is dissolved in 250ml of 1% acetic acid solution by volume, and the temperature is raised to 60°C. Phosphorous acid solution with a mass volume concentration of 0.25g / ml is added; 15ml of mass percentage is added 37% formaldehyde solution, stirred at 70℃ for 1h; pour the reaction solution into absolute ethanol to precipitate, filter, collect the precipitate, soak and wash twice with absolute ethanol, freeze-dry at -20℃ for 24h to obtain phosphorylation Chitosan
[0024] (2) Preparation of matrine / carboxymethyl chitosan / phosphorylated chitosan nanoparticle water dispersion: 5ml of matrine with a concentration of 1.5mg / ml (the chemical structure of matrine is as figure 1 Shown) The aqueous solution is mixed with 5 ml of the carboxymethyl chitosan aqueous solution with a concentration of 0.35 mg / ml, and the viscosity average ...
Embodiment 2
[0026] (1) Preparation of phosphorylated chitosan: 10g viscosity average molecular weight is 8.5×10 4 , Chitosan with a degree of deacetylation of 95% is dissolved in 500ml of acetic acid solution with a volume percentage of 1.5%, the temperature is raised to 75℃, and a phosphorous acid solution with a mass volume concentration of 0.5g / ml is added; 6ml is added with a mass percentage of 40% formaldehyde solution, stirred and reacted at 80℃ for 5.5h; Pour the reaction solution into absolute ethanol to precipitate, filter, collect the precipitate, soak and wash 3 times with absolute ethanol, freeze-dry at -30℃ for 48h to obtain phosphoric acid Chitosan;
[0027] (2) Preparation of matrine / carboxymethyl chitosan / phosphorylated chitosan nanoparticle water dispersion: 10ml of matrine aqueous solution with a concentration of 1.0mg / ml and 15ml of carboxymethyl with a concentration of 0.5mg / ml Mix the methyl chitosan aqueous solution, the viscosity average molecular weight of the carboxy...
Embodiment 3
[0029] (1) Preparation of phosphorylated chitosan: 8g viscosity average molecular weight is 2.2×10 5 , Chitosan with a degree of deacetylation of 92% is dissolved in 350ml of 1.2% acetic acid solution, heated to 65°C, added with a phosphorous acid solution with a mass volume concentration of 0.45g / ml; added 10ml with a mass percentage of 38% formaldehyde solution, stirred for 2h at 75℃; pour the reaction solution into absolute ethanol to precipitate, filter, collect the precipitate, soak and wash twice with absolute ethanol, freeze-dry at -10℃ for 38h to obtain phosphorylation Chitosan
[0030] (2) Preparation of matrine / carboxymethyl chitosan / phosphorylated chitosan nanoparticle water dispersion: 8ml of matrine aqueous solution with a concentration of 2.0mg / ml and 10ml of carboxymethyl with a concentration of 0.25mg / ml Mix the methyl chitosan aqueous solution, the viscosity average molecular weight of the carboxymethyl chitosan is 5.3×10 5 Under stirring conditions, add the abov...
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