CN110946134A - Pesticide preparation with polyurethane as carrier and preparation method thereof - Google Patents

Pesticide preparation with polyurethane as carrier and preparation method thereof Download PDF

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Publication number
CN110946134A
CN110946134A CN201911055055.1A CN201911055055A CN110946134A CN 110946134 A CN110946134 A CN 110946134A CN 201911055055 A CN201911055055 A CN 201911055055A CN 110946134 A CN110946134 A CN 110946134A
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polyurethane
pesticide
preparation
carrier
raw materials
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CN110946134B (en
Inventor
张志祥
朱启绽
张超群
闫超
王世英
马千里
王瑞飞
刘本菊
徐汉虹
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South China Agricultural University
CATAS Environment and Plant Protection Institute
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South China Agricultural University
CATAS Environment and Plant Protection Institute
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • A01N25/10Macromolecular compounds
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01GHORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00Protecting plants
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/24Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients to enhance the sticking of the active ingredients
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/561,2-Diazoles; Hydrogenated 1,2-diazoles
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Environmental Sciences (AREA)
  • Dentistry (AREA)
  • Engineering & Computer Science (AREA)
  • Plant Pathology (AREA)
  • Pest Control & Pesticides (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Agronomy & Crop Science (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a pesticide preparation with polyurethane as a carrier, which is prepared from the following raw materials: a pesticide active ingredient, polyurethane, chitosan and water; the polyurethane was made from: castor oil, isophorone diisocyanate, dibutyltin dilaurate, methyldiethanolamine, and glacial acetic acid. The preparation method comprises the following steps: weighing raw materials; mixing castor oil and isophorone diisocyanate, heating, stirring, adding dibutyltin dilaurate for reaction, and adding methyldiethanolamine for reaction; adding acetone for dissolving pesticide active ingredients to react, cooling, adding glacial acetic acid to neutralize, adding water to emulsify, and distilling to remove acetone; adding chitosan, heating and stirring to obtain the final product. The pesticide preparation takes polyurethane as a carrier, and the pesticide active ingredient is encapsulated in the carrier, so that the pesticide preparation can be effectively attached to plant leaves to form a pesticide film, the pesticide cost is reduced, the pesticide preparation also has good insecticidal activity, the pesticide dosage is reduced, and the effective utilization rate of the pesticide is improved.

Description

Pesticide preparation with polyurethane as carrier and preparation method thereof
Technical Field
The invention relates to the technical field of pesticides, in particular to a pesticide preparation taking polyurethane as a carrier and a preparation method thereof.
Background
The pesticide emulsifiable agent is the most commonly used dosage form in pesticide dosage forms. In the dosage form, the active ingredients exist in a molecular state, the pesticide effect is high, the property is stable, the use history of the missible oil is long, and the processing technology is mature, so the dosage form has the advantages of multiple varieties, high yield, wide application range, simple process, small equipment investment, simple and easy packaging, small formulation development difficulty and the like.
Although the pesticide emulsifiable concentrate has many advantages, the pesticide emulsifiable concentrate has the defects that a large amount of organic solvents such as xylene and toluene are used in the preparation process, the content of the organic solvents is generally 20-90%, and the solvents have the hazards of high toxicity, flammability, unsafe storage and transportation, easy phytotoxicity to plants, serious environmental pollution and the like. Meanwhile, the organic solvents can also cause harm to human bodies in the processes of processing, packaging and using of missible oil, and particularly, in the process of spraying pesticides, the organic solvents are sprayed into the natural environment, so that not only is the environment seriously polluted, but also the biological chronic poisoning is caused. In addition, various emulsifiers are used in the general pesticide preparation process, and the production cost is increased. Therefore, China always strives to reduce the dosage of high-toxicity pesticides and replace the high-toxicity pesticides with safe and environment-friendly novel pesticide varieties.
The polyurethane is a high molecular material, and the waterborne polyurethane is a novel polyurethane system which takes water as a dispersion medium instead of an organic solvent, has the advantages of no pollution, safety, reliability, excellent mechanical property, good compatibility, easy modification and the like, and can be widely applied to coatings, adhesives, fabric coatings and finishing agents, leather finishing agents, paper surface treating agents and fiber surface treating agents. The vegetable oil is a renewable resource and has wide sources, and the vegetable oil-based waterborne polyurethane is a research hotspot for modifying the waterborne polyurethane.
Chitosan (chitosan) is obtained by deacetylation of chitin (chitin) widely existing in the nature, the chemical name is polyglucosamine (1-4) -2-amino-B-D glucose, chitosan is firstly obtained by Rouget of the Law of 1859, the excellent performances of the natural polymer, such as biological functionality, compatibility, blood compatibility, safety, microbial degradability and the like, are widely concerned by various industries, and the chitosan has film forming property and better viscosity, so that the application research in various fields, such as medicine, food, chemical industry, cosmetics, water treatment, metal extraction and recovery, biochemical engineering, biomedical engineering and the like, is greatly advanced.
Therefore, how to prepare a novel pesticide preparation by using the vegetable oil-based waterborne polyurethane and the chitosan is a problem which needs to be solved urgently by the technical personnel in the field.
Disclosure of Invention
In view of the above, the present invention provides a pesticide preparation using polyurethane as a carrier and a preparation method thereof. The pesticide preparation takes cationic castor oil-based waterborne polyurethane as a carrier, does not add various emulsifiers or organic solvents, and can be easily attached to hydrophobic leaf surfaces, thereby ensuring the durability of pesticide effect.
In order to achieve the purpose, the invention adopts the following technical scheme:
a pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in percentage by weight: 0.01 to 1 percent of pesticide active ingredient, 0.1 to 20 percent of polyurethane, 0 to 10 percent of chitosan and the balance of water;
wherein the polyurethane is prepared from the following raw materials in percentage by weight: 50-55% of castor oil (hydroxyl value is 164mgKOH/g), 30-35% of isophorone diisocyanate, 0.15-0.20% of dibutyltin dilaurate, 8-10% of methyl diethanolamine and 4-5% of glacial acetic acid.
Further, the pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in percentage by weight: 0.1-0.5% of pesticide active ingredient, 10-15% of polyurethane, 1-5% of chitosan and the balance of water;
wherein the polyurethane is prepared from the following raw materials in percentage by weight: 51 to 53 percent of castor oil (hydroxyl value is 164mgKOH/g), 32 to 34 percent of isophorone diisocyanate, 0.16 to 0.19 percent of dibutyltin dilaurate, 9 to 10 percent of methyldiethanolamine and 4.2 to 4.8 percent of glacial acetic acid.
Furthermore, the pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in percentage by weight: 0.5% of pesticide active ingredient, 15% of polyurethane, 5% of chitosan and 79.5% of water;
wherein the polyurethane is prepared from the following raw materials in percentage by weight: 52.31% of castor oil (hydroxyl value is 164mgKOH/g), 33.99% of isophorone diisocyanate, 0.18% of dibutyltin dilaurate, 9.02% of methyldiethanolamine and 4.5% of glacial acetic acid.
Further, the pesticide active ingredient is any one of chlorantraniliprole, thiacloprid, rotenone, azadirachtin, indoxacarb, dinotefuran, sulfoxaflor, clothianidin, thiamethoxam, acetamiprid, nitenpyram or cypermethrin, and is preferably chlorantraniliprole.
The chlorantraniliprole has the further beneficial effects that the chlorantraniliprole has strong permeability, can be quickly absorbed by crops after being used, and can effectively protect the crops from being damaged; meanwhile, the compound pesticide also has strong activity of killing the larvae which are hatched initially, thereby greatly reducing the survival rate of pests; in addition, the high-efficiency activity of the pesticide is very strong and is about 100 times of that of other pesticides on the market; its drug effect is very durable, even in rainy day it will not lose efficacy.
Further, the polyurethane is cationic castor oil-based waterborne polyurethane.
The further beneficial effect is that the castor oil has hydroxyl in the molecular structure, and can improve the mechanical property of the film when used as the soft segment of the aqueous polyurethane resin, and the castor oil has good hydrophobic effect.
The invention also provides a preparation method of the pesticide preparation taking polyurethane as the carrier, which comprises the following steps:
(1) weighing the raw materials according to the weight percentage of the pesticide preparation;
(2) adding the pesticide active ingredient into acetone for dissolving to obtain a mixed solution A for later use;
(3) mixing castor oil and isophorone diisocyanate, heating to 75-80 ℃, stirring at a rotating speed of 200-400 r/min for 10-20 min, adding dibutyltin dilaurate to react for 10-20 min, and then adding methyldiethanolamine to react for 5-10 min under the stirring condition to obtain a mixed solution B;
(4) adding the mixed solution A obtained in the step (1) into the mixed solution B obtained in the step (3), continuously reacting for 2-3 h, stopping heating, cooling to 18-25 ℃, adding glacial acetic acid for neutralization reaction for 30-60 min, finally adding water for emulsification for 2-3 h, and distilling to remove acetone to obtain a polyurethane emulsion;
(5) and (4) adding chitosan into the polyurethane emulsion obtained in the step (4), heating to 25-50 ℃, and stirring at a rotating speed of 300-600 r/min for 30-60 min to obtain the pesticide preparation taking polyurethane as a carrier.
Further, in the step (2), the mass ratio of the volume of the acetone to the polyurethane is 1: 3-9.
The invention also provides a using method of the pesticide preparation taking polyurethane as the carrier, which comprises the following steps: the pesticide preparation is directly mixed with water for spraying through a sprayer, and the pesticide preparation is not suitable for spraying in rainy days so as to prevent a pesticide film attached to the leaves of crops from being washed by rainwater and sliding off.
According to the technical scheme, compared with the prior art, the invention discloses a pesticide preparation taking polyurethane as a carrier and a preparation method thereof, and the pesticide preparation has the following beneficial effects:
1. the invention takes cationic castor oil-based waterborne polyurethane as a carrier, and the pesticide active ingredient is encapsulated in the carrier so as to be difficult to decompose;
2. the invention takes water as solvent, replaces toxic organic solvent which is used in large amount in the traditional preparation process of missible oil, solves the pollution problem and is safe and friendly to the environment;
3. the invention utilizes the film forming property and the adhesiveness of chitosan to improve the adhesion effect of the pesticide active ingredients on the blades;
4. the invention does not contain any emulsifier and organic solvent, reduces the production cost and reduces the probability of phytotoxicity.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, the cationic castor oil-based waterborne polyurethane is prepared from the following raw materials by weight: 52.31g of castor oil (hydroxyl value is 164mgKOH/g), 33.99g of isophorone diisocyanate, 0.18g of dibutyltin dilaurate, 9.02g of methyldiethanolamine and 4.5g of glacial acetic acid.
Example 1
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.05g of chlorantraniliprole, 10g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 88.95g of water.
The preparation method comprises the following steps:
(1) weighing the raw materials;
(2) dissolving chlorantraniliprole in 90mL of acetone to obtain a mixed solution A for later use;
(3) adding castor oil and isophorone diisocyanate (IPDI) into a 500mL three-neck round-bottom flask provided with a mechanical stirring device, stirring at 78 ℃ for 10min at the rotating speed of 200r/min, adding a catalyst dibutyltin dilaurate (DBTDL) for reaction for 10min, adding Methyldiethanolamine (MDEA) under the stirring condition, and continuing the reaction for 10min to obtain a mixed solution B;
(4) adding the mixed solution A obtained in the step (1) into the mixed solution B obtained in the step (3), continuously reacting for 2h at 78 ℃, cooling to 20 ℃, adding glacial acetic acid, neutralizing for 30min, adding water for emulsifying for 2h, and distilling by using a rotary evaporator to remove acetone to obtain a stable castor oil-based waterborne polyurethane emulsion;
(5) and (3) placing the castor oil-based waterborne polyurethane emulsion obtained in the step (4) into a container, adding chitosan, and stirring at the temperature of 25 ℃ and at the rotating speed of 300r/min for 30min to obtain the chlorantraniliprole insecticide with the concentration of 0.05%.
Example 2
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.05g of chlorantraniliprole, 12g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 86.95g of water.
The preparation method comprises the following steps:
(1) weighing the raw materials;
(2) dissolving chlorantraniliprole in 90mL of acetone to obtain a mixed solution A for later use;
(3) adding castor oil and isophorone diisocyanate (IPDI) into a 500mL three-neck round-bottom flask provided with a mechanical stirring device, stirring at 80 ℃ at a rotating speed of 300r/min for 20min, adding a catalyst dibutyltin dilaurate (DBTDL) for reacting for 20min, adding Methyldiethanolamine (MDEA) under the stirring condition, and continuing to react for 5min to obtain a mixed solution B;
(4) adding the mixed solution A obtained in the step (1) into the mixed solution B obtained in the step (3), continuously reacting for 3h at 80 ℃, cooling to 25 ℃, adding glacial acetic acid, neutralizing for 60min, adding water for emulsifying for 3h, and distilling by a rotary evaporator to remove acetone to obtain stable castor oil-based waterborne polyurethane emulsion;
(5) and (3) placing the castor oil-based waterborne polyurethane emulsion obtained in the step (4) into a container, adding chitosan, and stirring for 60min at the temperature of 50 ℃ and the rotating speed of 500r/min to obtain the chlorantraniliprole insecticide with the concentration of 0.05%.
Example 3
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.05g of chlorantraniliprole, 15g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 83.95g of water.
The preparation method comprises the following steps:
(1) weighing the raw materials;
(2) dissolving chlorantraniliprole in 90mL of acetone to obtain a mixed solution A for later use;
(2) adding castor oil and isophorone diisocyanate (IPDI) into a 500mL three-neck round-bottom flask provided with a mechanical stirring device, stirring at 75 ℃ for 15min at the rotating speed of 400r/min, adding a catalyst dibutyltin dilaurate (DBTDL) for reacting for 15min, adding Methyldiethanolamine (MDEA) under the stirring condition, and continuing to react for 8min to obtain a mixed solution B;
(4) adding the mixed solution A obtained in the step (1) into the mixed solution B obtained in the step (3), continuously reacting for 2.5h at 75 ℃, cooling to 18 ℃, adding 1g of glacial acetic acid, neutralizing for 45min, adding water for emulsifying for 2.5h, and distilling by using a rotary evaporator to remove acetone to obtain a stable castor oil-based waterborne polyurethane emulsion;
(5) and (3) placing the castor oil-based waterborne polyurethane emulsion obtained in the step (4) into a container, adding chitosan, and stirring for 45min at the temperature of 35 ℃ and the rotating speed of 600r/min to obtain the chlorantraniliprole insecticide with the concentration of 0.05%.
Example 4
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.1g of chlorantraniliprole, 15g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 83.9g of water.
The preparation method is the same as that of the example 1, and the chlorantraniliprole insecticide with the concentration of 0.1 percent is obtained.
Example 5
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.1g of chlorantraniliprole, 15g of cationic castor oil-based waterborne polyurethane, 2.5g of chitosan and 82.4g of water.
The preparation method is the same as that of the example 1, and the chlorantraniliprole insecticide with the concentration of 0.1 percent is obtained.
Example 6
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.1g of chlorantraniliprole, 15g of cationic castor oil-based waterborne polyurethane, 5g of chitosan and 79.9g of water.
The preparation method is the same as that of the example 1, and the chlorantraniliprole insecticide with the concentration of 0.1 percent is obtained.
Example 7
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.25g of chlorantraniliprole, 15g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 83.75g of water.
The preparation method is the same as that of the example 1, and the chlorantraniliprole insecticide with the concentration of 0.25 percent is obtained.
Example 8
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.25g of chlorantraniliprole, 15g of cationic castor oil-based waterborne polyurethane, 2.5g of chitosan and 82.25g of water.
The preparation method is the same as that of the example 1, and the chlorantraniliprole insecticide with the concentration of 0.25 percent is obtained.
Example 9
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.25g of chlorantraniliprole, 15g of cationic castor oil-based waterborne polyurethane, 5g of chitosan and 79.75g of water.
The preparation method is the same as that of the example 1, and the chlorantraniliprole insecticide with the concentration of 0.25 percent is obtained.
Example 10
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.5g of chlorantraniliprole, 15g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 83.5g of water.
The preparation method is the same as that of the example 1, and the chlorantraniliprole insecticide with the concentration of 0.5 percent is obtained.
Example 11
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.5g of chlorantraniliprole, 15g of cationic castor oil-based waterborne polyurethane, 2.5g of chitosan and 82g of water.
The preparation method is the same as that of the example 1, and the chlorantraniliprole insecticide with the concentration of 0.5 percent is obtained.
Example 12
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.5g of chlorantraniliprole, 15g of cationic castor oil-based waterborne polyurethane, 5g of chitosan and 79.5g of water.
The preparation method is the same as that of the example 1, and the chlorantraniliprole insecticide with the concentration of 0.5 percent is obtained.
Example 13
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.05g of rotenone, 10g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 88.95g of water.
The preparation method is the same as that of example 1, and the rotenone insecticide with the concentration of 0.05 percent is obtained.
Example 14
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.05g of rotenone, 12g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 86.95g of water.
The preparation method is the same as that of example 1, and the rotenone insecticide with the concentration of 0.05 percent is obtained.
Example 15
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.05g of rotenone, 15g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 83.95g of water.
The preparation method is the same as that of example 1, and the rotenone insecticide with the concentration of 0.05 percent is obtained.
Example 16
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.1g of rotenone, 15g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 83.9g of water.
The preparation method is the same as that of the example 1, and the rotenone insecticide with the concentration of 0.1 percent is obtained.
Example 17
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.1g of rotenone, 15g of cationic castor oil-based waterborne polyurethane, 2.5g of chitosan and 82.4g of water.
The preparation method is the same as that of the example 1, and the rotenone insecticide with the concentration of 0.1 percent is obtained.
Example 18
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.1g of rotenone, 15g of cationic castor oil-based waterborne polyurethane, 5g of chitosan and 79.9g of water.
The preparation method is the same as that of the example 1, and the rotenone insecticide with the concentration of 0.1 percent is obtained.
Example 19
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.25g of rotenone, 15g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 83.75g of water.
The preparation method is the same as that of the example 1, and the rotenone insecticide with the concentration of 0.25 percent is obtained.
Example 20
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.25g of rotenone, 15g of cationic castor oil-based waterborne polyurethane, 2.5g of chitosan and 82.25g of water.
The preparation method is the same as that of the example 1, and the rotenone insecticide with the concentration of 0.25 percent is obtained.
Example 21
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.25g of rotenone, 15g of cationic castor oil-based waterborne polyurethane, 5g of chitosan and 79.75g of water.
The preparation method is the same as that of the example 1, and the rotenone insecticide with the concentration of 0.25 percent is obtained.
Example 22
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.5g of rotenone, 15g of cationic castor oil-based waterborne polyurethane, 1g of chitosan and 83.5g of water.
The preparation method is the same as that of the example 1, and the rotenone insecticide with the concentration of 0.5 percent is obtained.
Example 23
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.5g of rotenone, 15g of cationic castor oil-based waterborne polyurethane, 2.5g of chitosan and 82g of water.
The preparation method is the same as that of the example 1, and the rotenone insecticide with the concentration of 0.5 percent is obtained.
Example 24
The pesticide preparation with polyurethane as a carrier is prepared from the following raw materials in parts by weight: 0.5g of rotenone, 15g of cationic castor oil-based waterborne polyurethane, 5g of chitosan and 79.5g of water.
The preparation method is the same as that of the example 1, and the rotenone insecticide with the concentration of 0.5 percent is obtained.
Performance detection
1. Field efficacy test of different chlorantraniliprole insecticide products
The chlorantraniliprole insecticides prepared in examples 1-12 were respectively subjected to field efficacy tests, the application method was conventional spraying, water was used as a control group, Spodoptera frugiperda was used as a test object, corn was used as a test crop, the three tests were repeated, the number of live insects was counted before application, the active ingredient was applied at a dose of 3.99 g/mu, the number of live insects was counted 5 days, 7 days and 15 days after application, and the population decline rate and control effect were calculated.
The oral cavity decline rate (%) (number of live insects before treatment-number of live insects after treatment)/number of live insects before treatment x 100%;
control effect (%) [1- (number of live insects after drug treatment x number of live insects before drug treatment in control area)/(number of live insects before drug treatment x number of live insects after drug treatment in control area) ] × 100%; the test results are shown in tables 1 to 3.
TABLE 1 field efficacy test results 5 days after application of chlorantraniliprole insecticide
Figure BDA0002256331560000111
Figure BDA0002256331560000121
TABLE 2 field efficacy test results 7 days after chlorantraniliprole application
Figure BDA0002256331560000122
Figure BDA0002256331560000131
TABLE 3 field efficacy test results 15 days after chlorantraniliprole application
Figure BDA0002256331560000132
Figure BDA0002256331560000141
As can be seen from tables 1 to 3, compared with the control group, the pesticide preparations prepared in examples 1 to 12 greatly improve the insect population regression rate and the control effect, the insect population regression rate can reach 97.10% at most, and the control effect can reach 97.90% at most. The pesticide preparation using the polyurethane as the carrier has good insecticidal effect.
The embodiment shows that the higher the content of the polyurethane, the better the adhesiveness of the medicament, and the more the amount of the medicament attached to crops, the better the control effect; the higher the chitosan content is, the better the adhesion of the medicament is, the more the medicament amount is attached to crops, and the better the control effect is.
2. Test of field drug effect of different rotenone insecticide products
The rotenone insecticides prepared in examples 13 to 24 were respectively subjected to field efficacy tests, the application method was conventional spraying, water was used as a control group, aphids were used as a test object, cabbage was used as a test crop, the tests were repeated three times, the number of live insects was counted before application, the active ingredient was applied at a dose of 3.6 g/mu, the number of live insects was counted 5 days, 7 days and 15 days after application, respectively, and the incidence of population decline and control effect were calculated.
The oral cavity decline rate (%) (number of live insects before treatment-number of live insects after treatment)/number of live insects before treatment x 100%;
control effect (%) [1- (number of live insects after drug treatment x number of live insects before drug treatment in control area)/(number of live insects before drug treatment x number of live insects after drug treatment in control area) ] × 100%; the test results are shown in tables 4 to 6.
TABLE 4 field efficacy test results after 5 days of application of rotenone insecticide
Figure BDA0002256331560000151
Figure BDA0002256331560000161
TABLE 5 field test results of pesticide effect 7 days after application of rotenone insecticide
Figure BDA0002256331560000162
Figure BDA0002256331560000171
TABLE 6 field test results of pesticide effect 15 days after application of rotenone insecticide
Figure BDA0002256331560000172
Figure BDA0002256331560000181
As can be seen from tables 4 to 6, compared with the control group, the pesticide preparations prepared in examples 13 to 24 have greatly improved insect population regression rate and control effect, the insect population regression rate can reach 98.72% at most, and the control effect can reach 98.84% at most. The pesticide preparation using the polyurethane as the carrier has good insecticidal effect.
The embodiment shows that the higher the content of the polyurethane, the better the adhesiveness of the medicament, and the more the amount of the medicament attached to crops, the better the control effect; the higher the chitosan content is, the better the adhesion of the medicament is, the more the medicament amount is attached to crops, and the better the control effect is.

Claims (10)

1. A pesticide preparation taking polyurethane as a carrier is characterized by being prepared from the following raw materials in percentage by weight: 0.01-1% of pesticide active ingredient, 0.1-20% of polyurethane, 0-10% of chitosan and the balance of water;
the polyurethane is prepared from the following raw materials in percentage by weight: 50-55% of castor oil, 30-35% of isophorone diisocyanate, 0.15-0.20% of dibutyltin dilaurate, 8-10% of methyl diethanolamine and 4-5% of glacial acetic acid.
2. The pesticide preparation taking polyurethane as a carrier according to claim 1 is characterized by being prepared from the following raw materials in percentage by weight: 0.1-0.5% of pesticide active ingredient, 10-15% of polyurethane, 1-5% of chitosan and the balance of water;
the polyurethane is prepared from the following raw materials in percentage by weight: 51-53% of castor oil, 32-34% of isophorone diisocyanate, 0.16-0.19% of dibutyltin dilaurate, 9-10% of methyl diethanolamine and 4.2-4.8% of glacial acetic acid.
3. The pesticide preparation taking polyurethane as a carrier according to claim 1 is characterized by being prepared from the following raw materials in percentage by weight: 0.5% of pesticide active ingredient, 15% of polyurethane, 5% of chitosan and 79.5% of water;
the polyurethane is prepared from the following raw materials in percentage by weight: 52.31% of castor oil, 33.99% of isophorone diisocyanate, 0.18% of dibutyltin dilaurate, 9.02% of methyl diethanolamine and 4.5% of glacial acetic acid.
4. The pesticide preparation using polyurethane as a carrier according to any one of claims 1 to 3, wherein the pesticide active ingredient is any one of chlorantraniliprole, thiacloprid, rotenone, azadirachtin, methomyl, dinotefuran, sulfoxaflor, clothianidin, thiamethoxam, acetamiprid, nitenpyram or cypermethrin.
5. The pesticide preparation with polyurethane as a carrier according to any one of claims 1 to 3, characterized in that the polyurethane is cationic castor oil-based aqueous polyurethane.
6. A preparation method of a pesticide preparation taking polyurethane as a carrier is characterized by comprising the following steps:
(1) weighing the raw materials according to the weight percentage of the pesticide preparation of any one of claims 1 to 5;
(2) adding the pesticide active ingredient into acetone for dissolving to obtain a mixed solution A for later use;
(3) mixing castor oil and isophorone diisocyanate, heating, stirring for 10-20 min, adding dibutyltin dilaurate to react for 10-20 min, and then adding methyldiethanolamine to react for 5-10 min under the stirring condition to obtain a mixed solution B;
(4) adding the mixed solution A obtained in the step (1) into the mixed solution B obtained in the step (3), continuously reacting for 2-3 h, stopping heating, cooling, adding glacial acetic acid for neutralization reaction for 30-60 min, finally adding water for emulsification for 2-3 h, and distilling to remove acetone to obtain a polyurethane emulsion;
(5) and (4) adding chitosan into the polyurethane emulsion obtained in the step (4), heating, and stirring for 30-60 min to obtain the pesticide preparation with polyurethane as a carrier.
7. The preparation method of the pesticide preparation with the polyurethane as the carrier according to claim 6, wherein in the step (2), the mass ratio of the volume of the acetone to the polyurethane is 1: 3-9.
8. The method for preparing a pesticide preparation with polyurethane as a carrier according to claim 6, wherein in the step (3), the temperature is raised to 75-80 ℃, and the rotation speed of stirring is 200-400 r/min.
9. The method for preparing the pesticide preparation with the polyurethane as the carrier according to the claim 6, wherein in the step (4), the cooling is carried out to 18-25 ℃.
10. The method for preparing a pesticide preparation with polyurethane as a carrier according to claim 6, wherein in the step (5), the temperature is raised to 25-50 ℃, and the rotation speed of stirring is 300-600 r/min.
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