CN112425610A - Preparation system and application of pesticide suspending agent for preventing and treating kaffir lily leaf spot disease - Google Patents
Preparation system and application of pesticide suspending agent for preventing and treating kaffir lily leaf spot disease Download PDFInfo
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Abstract
The invention relates to a preparation system and application of a controlled-release pesticide suspending agent for preventing and treating kaffir lily leaf spot. A controlled-release pesticide suspending agent for preventing and treating leaf spot of kaffir lily comprises the following components in parts by weight: 20-40 parts of composite nano porous carbon particles, 5-8 parts of polyethylene glycol, 2-5 parts of sorbitol, 2-5 parts of xanthan gum, 0.1-0.5 part of propyl p-hydroxybenzoate, 5-8 parts of soluble starch and 30-50 parts of deionized water. The controlled-release pesticide suspending agent prepared by the invention is suitable for preventing and controlling leaf spot of kaffir lily and scale insects, can kill the kaffir lily and scale insects in a double way, is thorough in killing, has long action time and causes little pollution to the environment.
Description
Technical Field
The invention belongs to the technical field of pesticides, and particularly relates to a preparation system and application of a controlled-release pesticide suspending agent for preventing and treating kaffir lily leaf spot.
Background
Kaffir lily, also known as lycoris radiata and lycoris maxima, is a perennial herb of kaffir of lycoridaceae, belongs to ornamental flowers and is native to south africa. The flowering period is as long as 30-50 days, the flowers are mainly winter and spring, the flowers also bloom from the first day to the second day, the flowers are not strong, the flowers are semi-yin plants, the flowers like cool and are not high-temperature, the clivia miniata has high ornamental value, and China often pots in a greenhouse for ornamental. The variety of the Chinese medicinal composition comprises clivia miniata, clivia citrifolia and the like, and the Chinese medicinal composition is cultivated in greenhouses in various regions and has various colors. However, the occurrence of leaf spot of kaffir lily during cultivation greatly affects the ornamental value of kaffir lily. Kaffir lily leaf spot also infects other healthy kaffir lily, and brings huge economic loss. The kaffir lily leaf spot is very easy to occur when being seriously damaged by scale insects, and has certain drug resistance to the existing drugs. Therefore, a novel drug for dual control of kaffir lily leaf spot and scale insect is required to be searched.
Disclosure of Invention
In order to achieve the purpose, the invention provides a preparation system and application of a controlled-release pesticide suspending agent for preventing and treating kaffir lily leaf spot, and solves the defects of increasingly poor prevention and treatment effect and short drug action time caused by serious drug resistance due to long-term use of the existing drugs. The invention realizes the specific control effect on the leaf spot of the kaffir lily, can kill pathogenic bacteria and also kill scale insects causing the leaf spot of the kaffir lily, can continuously release medicaments, achieves the control effect which can be acted for a long time by one-time spraying, and is beneficial to improving the ornamental value and the economical efficiency of the kaffir lily.
The invention is realized by the following technical scheme:
the controlled-release pesticide suspending agent for preventing and treating leaf spot of kaffir lily is characterized by comprising the following components in parts by weight: 20-40 parts of composite nano porous carbon particles, 5-8 parts of polyethylene glycol, 2-5 parts of sorbitol, 2-5 parts of xanthan gum, 0.1-0.5 part of propyl p-hydroxybenzoate, 5-8 parts of starch and 30-50 parts of deionized water.
Further, the composite nano porous carbon particles comprise the following components in parts by weight: 20-25 parts of nanoporous carbon, 10-15 parts of medicinal material extracting solution, (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone, 0.05-0.1 part of conotoxin and 10-15 parts of modified chitosan nanogel; the medicinal material extracting solution is prepared from 5-10 parts of nux vomica, 5-10 parts of giant knotweed, 5-8 parts of common cnidium fruit and 10-15 parts of cinnamomum camphora.
further, the (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone is prepared by the following method:
(1) dissolving 2-oxazole benzene-4-formaldehyde and acetophenone in ethanol, and adding Fe3O4MNPs @ spring-Cu is refluxed for 15-30min, and the reaction is monitored by TLC to obtain reaction liquid;
(2) diluting the reaction solution in step (1) with 50-60 deg.C ethanol, and adding Fe by external magnet3O4MNPs @ Serine-Cu is separated from the reaction liquid to obtain residual reaction liquid, the residual reaction liquid is cooled to room temperature, crystals are separated out, the crystals are collected by filtration, washed by ethanol with the temperature of minus 10 to 0 ℃, and dried to obtain (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone.
Further, in the preparation method, 2-oxazole benzene-4-formaldehyde, acetophenone, ethanol and Fe3O4The mass ratio of MNPs @ spring-Cu is as follows: 10g to 12g to 40-50g to 4-6 g.
Further, said Fe3O4MNPs @ spring-Cu is prepared by the following method:
(1) preparation of Fe Using conventional Co-precipitation techniques3O4MNPs, followed by Fe3O4Adding MNPs into deionized water, ultrasonically dispersing at 30-45kHz for 30-40min, then adding serine, stirring at 50-60 ℃ at the rotating speed of 800-1000rmp for 6-8h, cooling to room temperature, and collecting newly generated Fe by a magnetic separation method3O4MNPs @ Serine, washed by deionized water, and dried for 8-10h at 80-90 ℃ in vacuum to obtain dried Fe3O4MNPs@Serine；
(2) Drying the Fe3O4Adding MNPs @ Serine into ethanol, ultrasonically dispersing at room temperature of 20-30kHz for 30-40min, and adding Cu (NO)3)2·3H2O, stirring for 24 hours at the temperature of 60-70 ℃ and the rotating speed of 800-3O4The reaction solution of MNPs @ Serine-Cu is cooled to room temperature, and Fe is collected by an external magnet separation method3O4MNPs @ Serine-Cu, washing with ethanol solution, and drying at 70-80 deg.C for 6-8h to obtain catalyst Fe3O4MNPs@Serine-Cu 。
Further, said Fe3O4Fe in preparation method of MNPs @ Serine-Cu3O4MNPs serine Cu (NO)3)2·3H2The weight ratio of O is: 10-12g, 15-17g, 18-20 g.
Further, the modified chitosan nano gel comprises the following components in parts by weight: 10-12 parts of chitosan, 4-8 parts of sodium dodecyl propionate and 2-5 parts of betaine.
Further, the modified chitosan nano gel is prepared by the following steps:
(1) dissolving chitosan in 3-5% acetic acid water solution to obtain 1.6-1.8g/L chitosan solution, and adjusting pH to 4.0-6.0 to obtain weakly acidic chitosan solution;
(2) adding sodium dodecyl propionate and betaine into the weakly acidic chitosan solution, stirring at the rotating speed of 800-;
(3) adding 1-1.5 times of 0.6g/L sodium tripolyphosphate aqueous solution into the alkaline reaction solution, stirring at the rotating speed of 800-1000rmp for 0.5-2h, and dialyzing in Phosphate Buffer Solution (PBS) with pH of 6.0-8.0 for 2-3 days to obtain modified chitosan nanogel;
further, the controlled-release pesticide suspending agent is prepared by the following steps:
(1) removing mildew, worm damage and impurities of the raw medicinal materials such as nux vomica, polygonum cuspidatum, fructus cnidii, cinnamomum camphora crushed leaves and the like, then putting the raw medicinal materials into a slicing machine for chopping, then putting the raw medicinal materials into a grinding machine for grinding into powder, then putting the powder into an ethanol solvent, adding potassium carbonate, stirring at the rotating speed of 1000-1500rmp, heating to 60-80 ℃, filtering after 4-5 hours to obtain filtrate, and concentrating to obtain a medicinal material extracting solution;
(2) mixing the medicinal material extract, (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone, conotoxin and nano porous carbon, and stirring at 50-60 ℃ at the rotating speed of 800-;
(3) and pouring the modified chitosan nanogel into the porous carbon nanocapsule core, uniformly stirring, and adding deionized water for dispersion to obtain the composite porous carbon nanocapsule particles.
(4) Mixing the composite nano porous carbon particles, polyethylene glycol, sorbitol, xanthan gum, propyl p-hydroxybenzoate, starch and deionized water, stirring at 40-50 ℃ at the rotating speed of 1000-1200rmp for 1-2h, and then cooling to room temperature to obtain the controlled-release pesticide suspending agent.
Furthermore, the preparation system of the preparation method of the controlled-release pesticide suspending agent comprises a slicing machine, a discharge hole of the slicing machine is communicated with a feed hole of a grinding machine, a discharge hole of the grinding machine is communicated with a first feed hole of a first stirring machine, a discharge hole of the first stirring machine is communicated with a feed hole of a thickener, a filter membrane is further arranged between the discharge hole of the first stirring machine and the feed hole of the thickener, a discharge hole of the thickener is communicated with a first feed hole of a second stirring machine, a liquid discharge hole is formed in the bottom of the second stirring machine, and a discharge hole of.
The prepared controlled-release pesticide suspending agent can be applied to preventing and treating leaf spot of kaffir lily.
The controlled-release pesticide suspending agent prepared by the invention has a special effect of preventing and treating the leaf spot disease of kaffir lily, can kill pathogenic bacteria and attract and kill scale insects causing the leaf spot disease of kaffir lily, has double prevention and treatment effects, is thorough and efficient, low in dosage, small in environmental pollution, capable of continuously releasing the pesticide for a long time, free of spraying the pesticide for multiple times and good in prevention and treatment effect in a long time. In addition, when the active ingredient (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone is prepared, the reaction condition is mild, the operation is simple and convenient, the reaction time is extremely short, the yield is up to 95 percent, the designed catalyst can be recycled, almost no by-product is generated, the reaction is clean and green, and the environment is protected.
Drawings
FIG. 1 is a hydrogen spectrum of (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-one;
FIG. 2 is a carbon spectrum of (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-one;
FIG. 3 is Fe3O4SEM picture of MNPs @ spring-Cu;
FIG. 4 is Fe3O4TEM image of MNPs @ Serine-Cu;
fig. 5 is a diagram of a system for preparing a controlled release pesticide suspension.
Detailed Description
The technical solutions of the present invention are further described in detail with reference to specific examples so that those skilled in the art can better understand the present invention and can implement the present invention, but the examples are not intended to limit the present invention.
Example 1
1. Catalyst Fe3O4Preparation of MNPs @ Serine-Cu
(1) Preparation of Fe Using conventional Co-precipitation techniques3O4MNPs10g, and Fe3O4Adding MNPs into deionized water, ultrasonically dispersing at 30kHz for 30min, then adding 15g of serine, stirring at 50 ℃ at the rotating speed of 800rmp for 6h, cooling to room temperature, and collecting newly generated Fe by a magnetic analysis method3O4MNPs @ Serine, washed by deionized water and dried for 8 hours at 80 ℃ in vacuum to obtain dried Fe3O4MNPs@Serine；
(2) Drying the Fe3O4Adding MNPs @ Serine into ethanol, ultrasonically dispersing at room temperature of 20kHz for 30min, and adding Cu (NO)3)2·3H2O18 g, stirred at 60 ℃ for 24h at a rotating speed of 800rmp to obtain Fe-containing iron3O4The reaction solution of MNPs @ Serine-Cu is cooled to room temperature, and Fe is collected by an external magnet separation method3O4MNPs @ Serine-Cu, and is washed by 50% ethanol, and is dried for 6h in a drying process at the temperature of 70 ℃, thus obtaining the catalyst Fe3O4MNPs@Serine-Cu。
2. Preparation of (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-one
(1) Dissolving 10g of 2-oxazole benzene-4-formaldehyde and 12g of acetophenone in 40g of ethanol, and then adding Fe3O4MNPs @ spring-Cu 4g is refluxed for 15min, and the completion of the reaction is monitored by TLC to obtain a reaction solution;
(2) diluting the reaction solution in step (1) with 50 ℃ ethanol, and adding Fe by an external magnet3O4MNPs @ Serine-Cu is separated from the reaction liquid to obtain residual reaction liquid, the residual reaction liquid is cooled to room temperature, crystals are separated out, the crystals are collected by filtration, washed by ethanol at 0 ℃ and dried to obtain (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone.
3. Preparation of modified chitosan nanogel
(1) Dissolving 10g of chitosan into 3% volume fraction acetic acid aqueous solution to obtain 1.6g/L chitosan solution, and then adjusting the pH value to 6.0 to obtain weakly acidic chitosan solution;
(2) adding 4g of sodium dodecyl propionate and 2g of betaine into a weakly acidic chitosan solution, stirring at the rotating speed of 800rmp for 6 hours, and adjusting the pH value to 10.0 by using an NaOH aqueous solution to obtain an alkaline reaction solution;
(3) adding 1 volume time of 0.6g/L sodium tripolyphosphate aqueous solution into the alkaline reaction solution, stirring at the rotating speed of 800rmp for 0.5h, and dialyzing in Phosphate Buffer Solution (PBS) with pH of 8.0 for 2 days to obtain modified chitosan nanogel;
4. preparation steps of controlled-release pesticide suspending agent
(1) Removing mildew, worm damage and impurities from raw medicinal materials such as 5g of nux vomica, 5g of giant knotweed, 5g of common cnidium fruit, 5g of cinnamomum camphora crushed leaves and the like, then putting the raw medicinal materials into a slicing machine for chopping, then putting the raw medicinal materials into a grinder for grinding into powder, then putting the powder into an ethanol solvent, adding 1g of potassium carbonate, stirring and heating the mixture to 60 ℃ at the rotating speed of 1000rmp, filtering the mixture after 4 hours to obtain filtrate, and concentrating the filtrate to obtain a medicinal material extracting solution;
(2) mixing 10g of medicinal material extracting solution, (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone 15g, conotoxin 0.05g and nano porous carbon 20g, stirring at 50 ℃ at the rotating speed of 800rmp for 2h, and screening out the shell core of the nano porous carbon;
(3) and pouring 10g of modified chitosan nano gel into a nano porous carbon shell core, uniformly stirring, and adding deionized water for dispersion to obtain the composite nano porous carbon particles.
(4) Mixing 20g of composite nano porous carbon particles, 5g of polyethylene glycol, 2g of sorbitol, 2g of xanthan gum, 0.1g of propyl p-hydroxybenzoate, 5g of starch and 30g of deionized water, stirring at 40 ℃ for 1h at the rotating speed of 1000rmp, and then cooling to room temperature to obtain the controlled-release pesticide suspending agent.
As shown in FIG. 5, a preparation system using the preparation method comprises a slicer 1, a slicer outlet 102 is communicated with a grinder inlet 201, a grinder outlet 202 is communicated with a first mixer inlet 301, a first mixer outlet 302 is communicated with a thickener inlet 401, a filter membrane 7 is further arranged between the first mixer outlet 302 and the thickener inlet 401, a thickener outlet 402 is communicated with a second mixer first inlet 501, a liquid outlet 503 is arranged at the bottom of the second mixer, and a second mixer outlet 502 is communicated with a third mixer first inlet 601.
When in use, the crushed nux vomica, giant knotweed rhizome, common cnidium fruit and cinnamomum camphora leaves enter a slicer 1 from a slicer inlet 101 to be chopped, then enter a grinder 2 from a slicer inlet 102 and a grinder inlet 201 to be ground into powder, then enter a first stirrer 3 from a grinder outlet 202 and a first stirrer first inlet 301, ethanol and potassium carbonate are added from a first stirrer second inlet 303, after stirring is finished, enter a concentrator 4 from a first stirrer second inlet 302, a filter membrane 7 and a concentrator inlet 401, after concentration is finished, the concentrated solution enters a second stirrer 5 from a concentrator outlet 402 and a second stirrer first inlet 501, and (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone is added from a second stirrer second inlet 504, Conotoxin and nano porous carbon, after stirring, continuously adding modified chitosan nanogel from a second feeding hole 504 of a second stirrer, after stirring again, adding deionized water from the second feeding hole 504 of the second stirrer for dispersion, after dispersion, discharging waste liquid through a liquid discharge hole 503 of the second stirrer, allowing the obtained composite nano porous carbon particles to enter a third stirrer 6 through a second discharging hole 502 of the second stirrer and a feeding hole 601 of the third stirrer, adding polyethylene glycol, sorbitol, xanthan gum, propyl p-hydroxybenzoate, starch and deionized water from a second discharging hole 602 of the third stirrer, and after stirring, allowing the composite nano porous carbon particles to flow out from a discharging hole 603 of the third stirrer to obtain the controlled-release pesticide suspending agent.
The obtained controlled-release pesticide suspending agent is applied to preventing and treating leaf spot of kaffir lily.
Example 2
1. Catalyst Fe3O4Preparation of MNPs @ Serine-Cu
(1) Preparation of Fe Using conventional Co-precipitation techniques3O4MNPs11g, and Fe3O4Adding MNPs into deionized water, ultrasonically dispersing at 40kHz for 35min, then adding 16g of serine, stirring at 55 ℃ at 900rmp for 7h, cooling to room temperature, and collecting newly generated Fe by magnetic analysis3O4MNPs @ Serine, washed with deionized water, and dried at 85 ℃ for 9h in vacuum to obtain dried Fe3O4MNPs@Serine；
(2) Drying the Fe3O4Adding MNPs @ Serine into ethanol, ultrasonically dispersing at 25kHz for 35min at room temperature, and adding Cu (NO)3)2·3H2O19 g, stirring at 65 ℃ for 24h at the rotating speed of 900rmp to obtain Fe-containing solution3O4MNPs@Serine-Cu reaction solution, cooling to room temperature, and collecting Fe by external magnet separation method3O4MNPs @ Serine-Cu, and is washed by 50% ethanol, and is dried for 7 hours in the drying process at the temperature of 75 ℃, thus obtaining the catalyst Fe3O4MNPs@Serine-Cu。
2. Preparation of (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-one
(1) Dissolving 10g of 2-oxazole benzene-4-formaldehyde and 12g of acetophenone in 45g of ethanol, and then adding Fe3O4MNPs @ spring-Cu 5g is refluxed for 25min, and the completion of the reaction is monitored by TLC to obtain a reaction solution;
(2) diluting the reaction solution in step (1) with 55 deg.C ethanol, and adding Fe by external magnet3O4MNPs @ Serine-Cu is separated from the reaction liquid to obtain residual reaction liquid, the residual reaction liquid is cooled to room temperature, crystals are separated out, the crystals are collected by filtration, washed by ethanol with the temperature of minus 5 ℃ and dried to obtain (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone.
3. Preparation of modified chitosan nanogel
(1) Dissolving 11g of chitosan into an acetic acid aqueous solution with the volume fraction of 4% to obtain a chitosan solution with the mass concentration of 1.7g/L, and then adjusting the pH value to 5.0 to obtain a weakly acidic chitosan solution;
(2) adding 6g of sodium dodecyl propionate and 3g of betaine into a weakly acidic chitosan solution, stirring at the rotating speed of 900rmp for 7 hours, and adjusting the pH value to 9.0 by using an NaOH aqueous solution to obtain an alkaline reaction solution;
(3) adding 0.6g/L sodium tripolyphosphate aqueous solution with the volume of 1.3 times of that of the alkaline reaction solution, stirring at the rotating speed of 900rmp for 1h, and dialyzing in Phosphate Buffer Solution (PBS) with the pH value of 7.0 for 2.5 days to obtain modified chitosan nanogel;
4. preparation of controlled release pesticide suspension
(1) Removing mildew, worm damage and impurities from raw medicinal materials such as 7g of nux vomica, 7g of giant knotweed, 6g of common cnidium fruit, 12g of cinnamomum camphora crushed leaves and the like, then putting the raw medicinal materials into a slicing machine for chopping, then putting the raw medicinal materials into a grinder for grinding into powder, then putting the powder into an ethanol solvent, adding 2g of potassium carbonate, stirring and heating the mixture to 70 ℃ at the rotating speed of 900rmp, filtering the mixture after 4.5 hours to obtain filtrate, and concentrating the filtrate to obtain a medicinal material extracting solution;
(2) mixing 13g of medicinal material extracting solution, (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone 18g, conotoxin 0.08g and nano porous carbon 23g, stirring at the temperature of 55 ℃ at the rotating speed of 900rmp for 3h, and screening out a nano porous carbon shell core;
(3) and pouring 12g of modified chitosan nanogel into the porous carbon nanocapsule core, uniformly stirring, and adding deionized water for dispersion to obtain the composite porous carbon nanocapsule particles.
(4) 30g of composite nano porous carbon particles, 7g of polyethylene glycol, 3g of sorbitol, 4g of xanthan gum, 0.3 g of propyl p-hydroxybenzoate, 6g of starch and 40g of deionized water are mixed, stirred at the temperature of 45 ℃ at the rotating speed of 1100rmp for 1.5h, and then cooled to room temperature, so as to obtain the controlled-release pesticide suspending agent.
The obtained controlled-release pesticide suspending agent is applied to preventing and treating leaf spot of kaffir lily.
Example 3
1. Catalyst Fe3O4Preparation of MNPs @ Serine-Cu
(1) Preparation of Fe Using conventional Co-precipitation techniques3O4MNPs12g, and Fe3O4Adding MNPs into deionized water, ultrasonically dispersing at 45kHz for 40min, then adding 17g of serine, stirring at 60 ℃ at the rotating speed of 1000rmp for 8h, cooling to room temperature, and collecting newly generated Fe by a magnetic analysis method3O4MNPs @ Serine, washed by deionized water and dried for 10h at 90 ℃ in vacuum to obtain dried Fe3O4MNPs@Serine；
(2) Drying the Fe3O4Adding MNPs @ Serine into ethanol, ultrasonically dispersing at room temperature of 30kHz for 40min, and adding Cu (NO)3)2·3H2O20 g, stirring at 70 ℃ for 24h at the rotating speed of 1000rmp to obtain Fe-containing iron3O4The reaction solution of MNPs @ Serine-Cu is cooled to room temperature, and Fe is collected by an external magnet separation method3O4MNPs @ Serine-Cu, and is washed by 50% ethanol, and is dried for 8 hours in a drying process at the temperature of 80 ℃, and the catalyst Fe is obtained3O4MNPs@Serine-Cu。
2. Preparation of (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-one
(1) Dissolving 10g of 2-oxazole benzene-4-formaldehyde and 12g of acetophenone in 50g of ethanol, and then adding Fe3O4MNPs @ spring-Cu 6g is refluxed for 30min, and the reaction is monitored by TLC to obtain reaction liquid;
(2) diluting the reaction solution in step (1) with ethanol at 60 deg.C, and adding Fe by external magnet3O4MNPs @ Serine-Cu is separated from the reaction liquid to obtain residual reaction liquid, the residual reaction liquid is cooled to room temperature, crystals are separated out, the crystals are collected by filtration, washed by ethanol with the temperature of minus 10 ℃, and dried to obtain (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone.
3. Preparation of modified chitosan nanogel
(1) Dissolving 12g of chitosan into an acetic acid aqueous solution with volume fraction of 5% to obtain a chitosan solution with mass concentration of 1.8g/L, and then adjusting the pH value to 6.0 to obtain a weakly acidic chitosan solution;
(2) adding 8g of sodium dodecyl propionate and 5g of betaine into a weakly acidic chitosan solution, stirring at the rotating speed of 1000rmp for 8 hours, and adjusting the pH value to 8.0 by using an NaOH aqueous solution to obtain an alkaline reaction solution;
(3) adding 0.6g/L sodium tripolyphosphate aqueous solution with the volume of 1.5 times of the alkaline reaction solution, stirring at the rotating speed of 1000rmp for 2h, and dialyzing in Phosphate Buffer Solution (PBS) with the pH value of 6.0 for 3 days to obtain modified chitosan nanogel;
4. preparation steps of controlled-release pesticide suspending agent
(1) Removing mildew, worm damage and impurities from raw medicinal materials such as 10g of nux vomica, 10g of giant knotweed, 8g of common cnidium fruit, 15g of cinnamomum camphora crushed leaves and the like, then putting the raw medicinal materials into a slicing machine for chopping, then putting the raw medicinal materials into a grinder for grinding into powder, then putting the powder into an ethanol solvent, adding 3g of potassium carbonate, stirring and heating the mixture to 80 ℃ at the rotating speed of 1500rmp, filtering the mixture after 5 hours to obtain filtrate, and concentrating the filtrate to obtain a medicinal material extracting solution;
(2) mixing 15g of medicinal material extracting solution, (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone 20g, conotoxin 0.1g and nano porous carbon 25g, and stirring at the temperature of 60 ℃ at the rotating speed of 1000rmp for 4 hours to obtain a nano porous carbon shell core;
(3) and pouring 15g of modified chitosan nano gel into the nano porous carbon shell core, uniformly stirring, and adding deionized water for dispersion to obtain the composite nano porous carbon particles.
(4) 40g of composite nano porous carbon particles, 8g of polyethylene glycol, 5g of sorbitol, 5g of xanthan gum, 0.5g of propyl p-hydroxybenzoate, 8g of starch and 50g of deionized water are mixed, stirred at the rotating speed of 1200rmp at the temperature of 50 ℃ for 2 hours, and then cooled to room temperature to obtain the controlled-release pesticide suspending agent.
The obtained controlled-release pesticide suspending agent is applied to preventing and treating leaf spot of kaffir lily.
Test example 1
For Fe obtained in example 1 of the present invention3O4MNPs @ spring-Cu, using electron microscopy and transmission electron microscopy for Fe catalyst3O4MNPs @ spring-Cu were scan evaluated (FIGS. 3 and 4). It can be seen from fig. 3 that the catalyst is spherical spheres with a diameter of 25 nm, and fig. 4 shows that the catalyst is almost monodisperse at 30 nm.
Test example 2
The (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-one obtained in example 1 of the present invention was structurally characterized and the data obtained were as follows:
Light yellow solid; mp: 58-62℃,Yield:95%; 1H NMR (400 MHz, CDCl3), δ, ppm: 8.03 (dd, J = 7.5, 1.5 Hz, 2H), 7.50(m, 4H), 7.47 (d, J = 15.7 Hz, 1H), 7.20 (d, 1H), 2.55 (s, 3H). 13C NMR (400 MHz, CDCl3), δ, ppm: 192.01, 154.26, 146.11, 137.99, 134.55, 128.70, 128.10, 125.35, 124.04, 122.44，14.19. HRMS(EI): m/z [M+Na]+ calcd for C8H6BrClNaO: 237.0826; found: 237.0892.
test example 3
The controlled-release pesticide suspending agent prepared in the embodiments 1 to 3 of the invention is used for preventing and treating the leaf spot of kaffir lily. The variety of the kaffir lily used in the experiment is kaffir lily, the kaffir lily is normally cultivated indoors, 240 pots of diseased kaffir lily are divided into 8 groups randomly at the initial stage of the disease of scale insects and leaf spot diseases, one group is used as a control group and is not treated, the rest groups are marked as A, B, C, D, E, F, G respectively, the plant leaves are sprayed with the combination liquid of 50 percent carbendazim 1000-fold liquid, 70 percent thiophanate 1000-fold liquid, 45 percent ambam 1000-fold liquid, 50 percent carbendazim 1000-fold liquid, 70 percent thiophanate 1000-fold liquid and 45 percent ambam 1000-fold liquid which are purchased in the market respectively, and the combination liquid is sprayed once every week and is used for three times continuously; 1000 times of the controlled release pesticide suspension prepared in example 1, 1000 times of the controlled release pesticide suspension prepared in example 2, 1000 times of the controlled release pesticide suspension prepared in example 3; spraying was done only once in the initial week.
After 3 months, the leaves were evaluated-data expressed as% efficacy against leaf spot and scale insects compared to untreated plants.
The experimental evaluation of 7 groups of kaffir lily recorded in the table shows that the one-time spraying effect of the pesticide suspending agent is better than that of the sprayed existing pesticide for 3-4 times, wherein the 1000-fold liquid of the pesticide suspending agent is compared with the 1000-fold liquid of 50% carbendazim, the 1000-fold liquid of 70% thiophanate wettable powder and the 1000-fold liquid of 50% amobam, the resistance effect on leaf spot is 30-40% higher, and the resistance effect on scale insects is 60-70% higher; compared with a combined solution of 50% carbendazim 1000-fold solution, 70% thiophanate 1000-fold solution and 50% amobam 1000-fold solution, the composition has the advantages that the resistance effect on leaf spot is 10% higher, and the resistance effect on scale insects is about 30% higher.
While the invention has been described in further detail with reference to specific embodiments thereof, it is not intended that the invention be limited to the specific embodiments thereof; for those skilled in the art to which the present invention pertains and related technologies, the extension, operation method and data replacement should fall within the protection scope of the present invention based on the technical solution of the present invention.
Claims (10)
1. The controlled-release pesticide suspending agent for preventing and treating leaf spot of kaffir lily is characterized by comprising the following components in parts by weight: 20-40 parts of composite nano porous carbon particles, 5-8 parts of polyethylene glycol, 2-5 parts of sorbitol, 2-5 parts of xanthan gum, 0.1-0.5 part of propyl p-hydroxybenzoate, 5-8 parts of starch and 30-50 parts of deionized water.
2. The controlled-release pesticide suspension according to claim 1, wherein the composite nanoporous carbon particles comprise the following components in parts by weight: 20-25 parts of nanoporous carbon, 10-15 parts of medicinal material extracting solution, (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone, 0.05-0.1 part of conotoxin and 10-15 parts of modified chitosan nanogel; the medicinal material extracting solution comprises the following components in parts by weight: 5-10 parts of nux vomica, 5-10 parts of giant knotweed, 5-8 parts of common cnidium fruit and 10-15 parts of camphor.
3. The controlled-release pesticidal suspension according to claim 2, wherein the chemical structural formula of (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-one is:
the controlled-release pesticidal suspension according to claim 2, wherein the (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-one is prepared by the following method:
(1) dissolving 2-oxazole benzene-4-formaldehyde and acetophenone in ethanol, and adding Fe3O4MNPs @ spring-Cu is refluxed for 15-30min, and the reaction is monitored by TLC to obtain reaction liquid;
(2) diluting the reaction solution in step (1) with 50-60 deg.C ethanol, and adding Fe by external magnet3O4MNPs @ Serine-Cu is separated from the reaction liquid to obtain residual reaction liquid, the residual reaction liquid is cooled to room temperature, crystals are separated out, the crystals are collected by filtration, washed by ethanol with the temperature of minus 10 to 0 ℃, and dried to obtain (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone.
4. (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-carboxylic acid as described in claim 4A process for the preparation of ketones, characterized in that Fe is used3O4MNPs @ spring-Cu is prepared by the following method:
(1) preparation of Fe Using conventional Co-precipitation techniques3O4MNPs, followed by Fe3O4Adding MNPs into deionized water, ultrasonically dispersing at 30-45kHz for 30-40min, then adding serine, stirring at 50-60 ℃ at the rotating speed of 800-1000rmp for 6-8h, cooling to room temperature, and collecting newly generated Fe by a magnetic separation method3O4MNPs @ Serine, washed by deionized water, and dried for 8-10h at 80-90 ℃ in vacuum to obtain dried Fe3O4MNPs@Serine；
(2) Drying the Fe3O4Adding MNPs @ Serine into ethanol, ultrasonically dispersing at room temperature of 20-30kHz for 30-40min, and adding Cu (NO)3)2·3H2O, stirring for 24 hours at the temperature of 60-70 ℃ and the rotating speed of 800-3O4The reaction solution of MNPs @ Serine-Cu is cooled to room temperature, and Fe is collected by an external magnet separation method3O4MNPs @ Serine-Cu, washing with ethanol solution, and drying at 70-80 deg.C for 6-8h to obtain catalyst Fe3O4MNPs@Serine-Cu。
5. The controlled-release pesticide suspension concentrate as claimed in claim 2, wherein the modified chitosan nanogel consists of the following components in parts by weight: 10-12 parts of chitosan, 4-8 parts of sodium dodecyl propionate and 2-5 parts of betaine.
6. The controlled-release pesticide suspension as claimed in claim 2, wherein the modified chitosan nanogel is prepared by the following steps:
dissolving chitosan in acetic acid water solution, and adjusting pH to 4.0-6.0 to obtain weakly acidic chitosan solution;
adding sodium dodecyl propionate and betaine into the chitosan solution, stirring for 6-8h at the rotating speed of 800-;
(3) adding sodium tripolyphosphate aqueous solution into the alkaline reaction solution, stirring at the rotating speed of 800-1000rmp for 0.5-2h, and dialyzing in Phosphate Buffer Solution (PBS) with the pH value of 6.0-8.0 for 2-3 days to obtain the modified chitosan nano gel.
7. A method of preparing using the controlled-release pesticidal suspension formulation of claim 1, characterized by comprising the steps of:
(1) removing mildew, worm damage and impurities of the raw medicinal materials such as nux vomica, polygonum cuspidatum, fructus cnidii, cinnamomum camphora crushed leaves and the like, then putting the raw medicinal materials into a slicing machine for chopping, then putting the raw medicinal materials into a grinding machine for grinding into powder, then putting the powder into an ethanol solvent, adding potassium carbonate, stirring at the rotating speed of 1000-1500rmp, heating to 60-80 ℃, filtering after 4-5 hours to obtain filtrate, and concentrating to obtain a medicinal material extracting solution;
(2) mixing the medicinal material extract, (E) -5- (2-methyl) -oxazole-vinyl-1-phenyl-1-ketone, conotoxin and nano porous carbon, and stirring at 50-60 ℃ at the rotating speed of 800-;
(3) and pouring the modified chitosan nanogel into the porous carbon nanocapsule core, uniformly stirring, and adding deionized water for dispersion to obtain the composite porous carbon nanocapsule particles.
And 8, (4) placing the composite nano porous carbon particles, polyethylene glycol, sorbitol, xanthan gum, propyl p-hydroxybenzoate, starch and deionized water in a stirrer, stirring at 40-50 ℃ for 1-2h at the rotating speed of 1000-1200rmp, and then cooling to room temperature to obtain the controlled-release pesticide suspending agent.
9. A preparation system using the preparation method of claim 8, which comprises a slicing machine, wherein a discharge hole of the slicing machine is communicated with a feed hole of a grinding machine, a discharge hole of the grinding machine is communicated with a first feed hole of a first stirring machine, a discharge hole of the first stirring machine is communicated with a feed hole of a thickener, a filter membrane is arranged between the discharge hole of the first stirring machine and the feed hole of the thickener, a discharge hole of the thickener is communicated with a first feed hole of a second stirring machine, a liquid discharge hole is arranged at the bottom of the second stirring machine, and a discharge hole of the second stirring machine is communicated with.
10. Use of the controlled release pesticide suspension concentrate for controlling leaf spot of kaffir lily as claimed in any one of claims 1 to 9.
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