Lignin-emamectin benzoate conjugate, preparation method, insecticide and application thereof
A technology of lignin and emamectin, which is applied in the field of lignin- emamectin conjugates to achieve the effects of wide adaptability, stable preparation, good resistance to photolysis and antioxidant properties
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[0053] The invention also discloses a preparation method of a lignin-amamectin sulfonate conjugate with anti-photolysis performance, comprising: using lignin as a carrier and coupling the pesticide emamectin sulfonate through chemical bonds to prepare emamectin benzoate-lignosulfonate Acid conjugates or emamectin benzoate-alkaline lignin conjugate pesticides.
[0054] In some of the technical solutions of the present invention, as a preference, in the preparation method, the lignin includes sodium lignosulfonate, alkaline lignin, calcium lignosulfonate and lignin-based derivatization produced lignin derivatives.
[0055]In some of the technical solutions of the present invention, as preferably, the following steps are included:
[0056] Sodium lignosulfonate SL is used as raw material to obtain modified lignosulfonic acid through sulfonation modification. The modified lignosulfonic acid is further converted into lignosulfonyl chloride by reacting with thionyl chloride, and th...
Embodiment 1
[0110] Example 1 Preparation of pesticide emamectin benzoate-lignosulfonic acid conjugate (EB-SL) using sodium lignosulfonate as carrier
[0111] (1) Preparation of lignosulfonic acid
[0112] Dissolve 10-30g of sodium lignosulfonate (SL) in distilled water, slowly add 2-10mL of 30% hydrogen peroxide under ice bath, then heat to 80°C, and stir at this temperature for 2h. Subsequently, 5-15 g of sodium sulfite and 1-6 g of formaldehyde are added to the above mixture, and the pH value is adjusted to 8-10. The resulting solution was continued to be heated to 80-90°C, stirred and reacted at this temperature for 3-6h, and then cooled to room temperature. Add 0.5-2mol / L hydrochloric acid solution dropwise to the cooled solution to promote the precipitation of lignosulfonic acid. The precipitate was washed with alcohol and then filtered, and the modified lignosulfonic acid obtained by filtering was dried at 80° C. to obtain a brown powder product.
[0113] (2) Preparation of ligni...
Embodiment 2
[0117] Example 2 Preparation of pesticide emamectin benzoate-alkaline lignin conjugate (EB-AL) with alkaline lignin as carrier
[0118] (1) Preparation of alkaline lignin acetic acid
[0119] Add 5-20g of basic lignin into 20-100mL of 40% sodium hydroxide aqueous solution, raise the temperature to 80-90°C and stir for 0.5-2h, then add 3-20g of chloroacetic acid, and reflux at 100°C-110°C for 3-6h . After the reaction, cool to room temperature, add absolute ethanol and let it settle overnight, filter with suction, wash the obtained black solid with distilled water, and obtain black solid alkaline lignin acetic acid after drying.
[0120] (2) Preparation of Alkaline Lignin Acetyl Chloride
[0121] Dissolve 1-5g of alkaline lignin acetic acid obtained in (1) in 10-50mL DMF, add SOCl under ice bath 2 2-10mL, rise to room temperature, and then react at room temperature for 2-6h. After the reaction is over, unreacted SOCl is removed under reduced pressure 2 , to obtain lignin ...
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