CN114365743A - Auxiliary composition for improving agricultural drug effect and preparation method thereof - Google Patents

Auxiliary composition for improving agricultural drug effect and preparation method thereof Download PDF

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Publication number
CN114365743A
CN114365743A CN202111661527.5A CN202111661527A CN114365743A CN 114365743 A CN114365743 A CN 114365743A CN 202111661527 A CN202111661527 A CN 202111661527A CN 114365743 A CN114365743 A CN 114365743A
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ether
oil
fatty acid
phosphatide
composition
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Inventor
董德臻
宋文勇
曹雄飞
王磊
范亚磊
秦婷婷
秦敦忠
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Jiangsu Sinvo Chemical Technology Co ltd
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Jiangsu Sinvo Chemical Technology Co ltd
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Priority to CN202311093089.6A priority Critical patent/CN117178983A/en
Priority to CN202111661527.5A priority patent/CN114365743A/en
Publication of CN114365743A publication Critical patent/CN114365743A/en
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N25/00—Biocides, 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
    • A01N25/30—Biocides, 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 characterised by the surfactants
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N25/00—Biocides, 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
    • A01N25/02—Biocides, 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 liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A01N25/06—Aerosols
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N25/00—Biocides, 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
    • A01N25/24—Biocides, 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
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N39/00—Biocides, pest repellants or attractants, or plant growth regulators containing aryloxy- or arylthio-aliphatic or cycloaliphatic compounds, containing the group or, e.g. phenoxyethylamine, phenylthio-acetonitrile, phenoxyacetone
    • A01N39/02—Aryloxy-carboxylic acids; Derivatives thereof
    • A01N39/04—Aryloxy-acetic acids; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/06—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings
    • A01N43/08—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings with oxygen as the ring hetero atom
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/74—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
    • A01N43/76—1,3-Oxazoles; Hydrogenated 1,3-oxazoles
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90—Biocides, 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
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION 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
    • A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
    • A01N57/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
    • A01N57/20—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals

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

Abstract

The invention discloses an auxiliary agent composition for improving agricultural drug effect and a preparation method thereof, wherein modified liposome and a mixture thereof are used as main active ingredients and are prepared by reasonable compounding combination and processing technology.

Description

Auxiliary composition for improving agricultural drug effect and preparation method thereof
Technical Field
The invention belongs to the field of pesticide adjuvants, and particularly relates to an adjuvant composition for improving agricultural drug effect and a preparation method thereof.
Background
Along with plant protection unmanned aerial vehicle's continuous development, plant protection mode of giving medicine to poor free of charge takes place very big change, compares traditional manual work and sprays the operation, flies to prevent that the operation has obvious advantage, nevertheless has a series of problems, wherein comparatively typical just flies to prevent liquid medicine drift, the inhomogeneous scheduling problem of spraying in the operation process.
The flying prevention operation height is higher, the water consumption per mu is reduced by 91% and above, the change of the parameters improves the utilization rate of the liquid medicine, but the traditional medicament is not applicable to the flying prevention operation any more. Based on this, a flying preventive aid has been developed, and conventional flying preventive aids mainly focus on inorganic salts, silicones, high molecular polymers, and the like. However, the above-mentioned flight control aids have the following problems: the liquid medicine that unmanned aerial vehicle sprayed concentration is high, the water yield is few, if add inorganic salt medicament, probably lead to the crop to appear the phytotoxicity, the fertilizer harm. And if the organic silicon type auxiliary agent can well improve the permeability of the pesticide and improve the insecticidal effect, the concentration of the liquid medicine sprayed by the unmanned aerial vehicle is high, and the high permeability easily causes phytotoxicity. And D-limonene has insecticidal and bactericidal effects, but the pesticide can affect pipelines of agricultural unmanned aerial vehicles and can reduce pesticide effects. Therefore, the flying prevention aid with ideal effect is lacked at present. And it needs to be further explained that the particle size of the liquid medicine sprayed by the unmanned aerial vehicle is very small, and in the actual spraying operation, the liquid medicine fog drops are easy to drift and lose due to the meteorological conditions, the liquid medicine system and the physiological and biochemical composition of crops and targets.
It is known that increasing the amount of drug received per unit area of crops, targets (insects, diseases, grasses) and the like is a direct factor affecting the efficacy of drugs. The pesticide effect directly affects the crop yield. Based on the lack of the flying prevention auxiliary agent with ideal effect at present, the dosage and the water quantity are generally increased in order to obtain the prevention and treatment effect, the pesticide effect can be guaranteed to a certain extent, the pesticide utilization rate is low, the necessary pesticide liquid quantity is increased, the mu input of agricultural materials is increased, the environment is accumulated (polluted), and meanwhile, the safety (pesticide residue) of crops (phytotoxicity) and final agricultural products is influenced.
Disclosure of Invention
1. Problems to be solved
The invention aims to provide a pesticide composition which has good weeding effect and is particularly suitable for flight control, and the composition can be effectively deposited on a target and generates good conduction effect in the flight control operation process;
the invention also aims to provide a preparation method of the pesticide composition.
2. Technical scheme
In order to solve the problems, the invention provides an auxiliary composition for improving the effect of agricultural medicines, which comprises the following components in parts by weight:
components Number of parts Preferred portionsNumber of
Modified vegetable oil 25～45 27～42
Modified liposome mixtures 5～11 5～5.5
Alcohol ether compound 5～11 4～4.5
Nonionic surfactant 6～8 7～7.5
Anionic surfactants 3～5 1～2
Deionized water 41～55 41～55
Further, the modified vegetable oil may be one or more of a methyl esterification modified vegetable oil, an ethoxylation modified vegetable oil, and an epoxidation modified vegetable oil.
Further, the vegetable oil may be one or more of soybean oil (such as soybean oil from Shandong Luhua group), rapeseed oil, palm oil (such as palm oil from Shandong kylin chemical Co., Ltd.), olive oil, coconut oil, mandarin oil (such as mandarin oil from Jiangxi Xinsen Natural plant oil Co., Ltd.), citronella oil, and turpentine oil (such as turpentine oil from Fujiangnuodde Biotech Co., Ltd.).
Further, the alcohol ether compound may be selected from one or more combinations of ethylene glycol, propylene glycol, diethylene glycol monobutyl ether, ethylene glycol butyl ether, propylene glycol methyl ether, diethylene glycol ethyl ether, ethylene glycol phenyl ether, ethylene glycol hexyl ether, diethylene glycol hexyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether, tripropylene glycol methyl ether, propylene glycol methyl ether acetate, propylene glycol propyl ether, dipropylene glycol propyl ether, propylene glycol butyl ether, dipropylene glycol butyl ether, tripropylene glycol butyl ether, propylene glycol phenyl ether, and n-propyl propionate. Further preferably, the alcohol ether compound may be one or more of ethylene glycol, diethylene glycol monobutyl ether, propylene glycol methyl ether acetate, propylene glycol propyl ether, dipropylene glycol propyl ether, propylene glycol butyl ether, dipropylene glycol butyl ether, and tripropylene glycol butyl ether.
Further, the nonionic surfactant may be one or more selected from polyoxyethylene type nonionic surfactants, polyhydric alcohol type nonionic surfactants, alkanolamide type nonionic surfactants, polyether type nonionic surfactants, and amine oxide type nonionic surfactants. Preferably, the nonionic surfactant can be one or more selected from fatty alcohol-polyoxyethylene ether, sorbitan, EO-PO block polyether, coco diethanol amide, alkylphenol polyoxyethylene ether phosphate and fatty alcohol ether ammonium sulfate.
Furthermore, the anionic surfactant can be selected from one or more of alpha-olefin sodium sulfonate, alpha-sulfo fatty acid methyl ester, oleoyl oxyethyl sodium sulfonate, N-oleoyl N-methyl taurate and diisooctyl succinate sodium sulfonate for compounding.
Further, the modified liposome is prepared by the following method:
1) modification of liposomes: heating and dehydrating the mixture of glycerophospholipid, sterol and polyhydroxy compound by using a catalyst; the temperature rise is 95-115 ℃, and the dehydration treatment time is 1-3 h;
2) then, heating to 121-151 ℃, and introducing ethylene oxide, wherein the maximum pressure is controlled not to exceed 1.4MPa in the ethylene oxide introducing process;
3) after the ethylene oxide is introduced, reacting at the temperature of 121-151 ℃ until the pressure is not changed, and finishing the reaction;
before the reaction is finished, the pressure needs to be controlled to be 1.12-1.25 MPa;
4) cooling (71-81 deg.C), adding neutralizing agent to adjust pH to 5-7;
5) respectively weighing the modified liposome, the fatty acid ester substances, the vitamins and the kasong solution, and mixing and stirring at 61-71 ℃ to obtain a modified liposome mixture;
the modified liposome is 89.2-97.8 wt%, the fatty acid ester substance is 2-11 wt%, the vitamin is 1.1-1.5 wt%, and the cason aqueous solution (mass concentration is 11%) is 1.1-1.3 wt%;
wherein the fatty acid ester substances are one or more of trimethylolpropane fatty acid ester, propylene glycol fatty acid ester, pentaerythritol fatty acid ester, polyethylene glycol fatty acid monoester, polyethylene glycol fatty acid diester, fatty acid polyoxyethylene ether fatty acid ester, polyglycerol fatty acid ester, sorbitan fatty acid and sucrose fatty acid ester.
Further, the polyhydroxy compound is a composition of alcohol and alcohol amine, and the alcohol is one or two of glycerol and glycol; the alcohol amine is one or two of diethanolamine and triethanolamine; the mass ratio of the alcohol to the alcohol amine is (55-95%): (5% to 45%).
Further, the glycerol phospholipid and one or more of soybean phospholipid, phosphatidic acid, sunflower phospholipid, rapeseed phospholipid, canola phospholipid, linseed phospholipid, castor oil phospholipid, soybean phospholipid hydrogenated derivative, phosphatidic acid hydrogenated derivative, sunflower phospholipid hydrogenated derivative, rapeseed phospholipid hydrogenated derivative, canola phospholipid hydrogenated derivative, linseed phospholipid hydrogenated derivative and castor oil phospholipid hydrogenated derivative are combined.
Further, the catalyst is one or a combination of several of sodium methoxide, potassium methoxide, sodium hydroxide and potassium hydroxide; the sterol is one or more of beta-sitosterol, beta-sitostanol, stigmasterol, stigmastanol, campesterol, campestanol, ergosterol, avenasterol, brassicasterol and cholesterol.
Further, the modified liposome is a transmembrane transport synergist SP-4821 in the engine chemical industry.
The preparation method of any one of the adjuvant compositions for improving the effect of agricultural drugs comprises the following steps:
oil phase preparation: the modified vegetable oil is contacted and mixed with an alcohol ether solvent, and then the anion and the nonionic surfactant which are mixed according to a certain proportion are contacted and mixed;
aqueous phase (mother liquor) configuration: contacting and mixing the modified liposome mixture with a nonionic surfactant;
injecting the oil phase into the water phase, and carrying out shearing treatment to obtain the synergistic composition; the shearing speed is 11111-21111 r/min; preferably, the shearing speed is (15111 +/-1111) r/min, and the shearing time is 11-15 min.
Further, the proportion of the anionic surfactant to the nonionic surfactant in the oil phase preparation process is (1.11-7.51): (8.51-11.11).
Further, the mass ratio of the nonionic surface active agent in the oil phase preparation process to the nonionic surface active agent in the water phase (mother liquor) preparation process is (1-3): (2-5).
Advantageous effects
The adjuvant composition for improving the agricultural drug effect is prepared by taking the modified liposome and the mixture thereof as main active ingredients through reasonable compounding combination and processing technology, has obvious synergistic effect on herbicides and has obvious synergistic effect on resistant weeds;
the auxiliary composition for improving the agricultural drug effect provided by the invention is used in a flight prevention scene, and can effectively adjust the particle size spectrum of the flying spray-proof droplets, so that the drifting can be effectively prevented in the drug application process, the deposition and detention of the liquid medicine droplets on the surface of a target are promoted, and the drug effect of the liquid medicine is improved.
The auxiliary agent composition for improving the agricultural pesticide effect can obviously promote the vegetative growth of crops, shows dark green leaf color, improves the chlorophyll content and increases the thousand-grain weight, and has a certain yield-increasing effect.
Detailed Description
Unless defined otherwise, in the present invention, all technical and scientific terms used have the same meaning as commonly understood by one of ordinary skill in the art to which the present invention belongs; as used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the present invention, those whose specific conditions are not specified in the examples are conducted under the conventional conditions or the conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The term "about" as used herein is used to provide the flexibility and inaccuracy associated with a given term, measure or value. The degree of flexibility of a particular variable can be readily determined by one skilled in the art.
As used herein, "11% phospholipid soybean oil", "31% phospholipid soybean oil", "51% phospholipid soybean oil" and "71% phospholipid soybean oil" mean soybean oil containing 11%, 31%, 51%, 71% lecithin; the aforementioned soybean oil can be purchased directly, and lecithin soybean oil as used in the following examples of preparation of modified liposome mixture is available from phospholipid science co.
Modified liposome mixture preparation example 1:
in this example, the preparation of the modified liposome mixture comprises the following specific steps:
1) 835g of soybean oil containing 11% of phospholipid, 131g of cholesterol, 25g of glycerol, 11g of diethanolamine and 6.78g of KOH (catalyst) are put into an alkoxylation reaction kettle, and nitrogen is replaced for three times; heating to 111 ℃ for dehydration for 1 h;
2) then, heating to 121-151 ℃, introducing 1261g of Ethylene Oxide (EO), wherein the maximum pressure in the ethylene oxide introduction process is less than 1.4 MPa;
3) after the ethylene oxide is introduced, curing is carried out at the temperature of 135 ℃, and when the pressure is close to 1.12MPa in the curing process, nitrogen is introduced to keep the pressure at 1.15-1.25 MPa;
when the pressure in the reaction kettle is kept unchanged, the reaction is finished, and the whole curing time is about 1-2 h;
4) vacuumizing for 1.5-1h, cooling to 71-81 ℃, adding a neutralizing agent HAc to adjust the pH to 5-7, and obtaining modified liposome;
5) 89.2g of modified liposome, 11g of Tween 81, 1.5g of vitamin E and 1.3g of kasong solution are weighed. Mixing and stirring at 71 deg.C for 31min to obtain transparent modified liposome composition, and obtaining modified liposome mixture (transmembrane transport synergist SP-4821 in engine chemical industry).
Modified liposome mixture preparation example 2:
in this example, the preparation of the modified liposome mixture comprises the following specific steps:
1) 835g of soybean oil containing 31% of phospholipid, 131g of cholesterol, 25g of glycerol, 11g of diethanolamine and 6.78g of KOH (catalyst) are put into an alkoxylation reaction kettle, and nitrogen is replaced for three times; heating to 111 ℃ for dehydration for 1 h;
2) then, raising the temperature to 111 ℃, and introducing 1261g of Ethylene Oxide (EO), wherein the maximum pressure in the ethylene oxide introduction process is less than 1.4 MPa;
3) after the ethylene oxide is introduced, curing is carried out at the temperature of 135 ℃, and when the pressure is close to 1.12MPa in the curing process, nitrogen is introduced to keep the pressure at 1.15-1.25 MPa;
when the pressure in the reaction kettle is kept unchanged, the reaction is finished, and the whole curing time is about 1-2 h;
4) vacuumizing for 1.5-1h, cooling to 71-81 ℃, adding a neutralizing agent HAc to adjust the pH to 5-7, and obtaining modified liposome;
5) 89.2g of modified liposome, 11g of Tween 81, 1.5g of vitamin E and 1.3g of kasong solution are weighed. Mixing and stirring at 71 deg.C for 31min to obtain transparent modified liposome composition, and obtaining modified liposome mixture.
Modified liposome mixture preparation example 3:
in this example, the preparation of the modified liposome mixture comprises the following specific steps:
1) 835g of soybean oil (equivalent to the mass ratio of lecithin to vegetable oil of 1:1) containing 51% of phospholipid, 131g of cholesterol, 25g of glycerol, 11g of diethanolamine and 6.78g of KOH (catalyst) are put into an alkoxylation reaction kettle, and nitrogen is replaced for three times; heating to 95 ℃ for dehydration for 1 h;
2) then, raising the temperature to 121 ℃, and introducing 1261g of Ethylene Oxide (EO), wherein the maximum pressure in the ethylene oxide introduction process is less than 1.4 MPa;
3) after the ethylene oxide is introduced, curing is carried out at the temperature of 121 ℃, and when the pressure is close to 1.12MPa in the curing process, nitrogen is introduced to keep the pressure at 1.15-1.25 MPa;
when the pressure in the reaction kettle is kept unchanged, the reaction is finished, and the whole curing time is about 1-2 h;
4) vacuumizing for 1.5-1h, cooling to 71-81 ℃, adding a neutralizing agent HAc to adjust the pH to 5-7, and obtaining modified liposome;
5) 89.2g of modified liposome, 11g of Tween 81, 1.5g of vitamin E and 1.3g of kasong solution are weighed. Mixing and stirring at 71 deg.C for 31min to obtain transparent modified liposome composition, and obtaining modified liposome mixture.
Modified liposome mixture preparation example 4:
in this example, the preparation of the modified liposome mixture comprises the following specific steps:
1) 811g of soybean oil containing 71% of phospholipid, 151g of cholesterol, 19.38g of glycerol, 14.62g of triethanolamine, 6g of monoethanolamine and 8g of KOH (catalyst) are put into an alkoxylation reaction kettle, and nitrogen is replaced for three times; heating to 115 ℃ and dehydrating for 1 h;
2) then, raising the temperature to 151 ℃, and introducing 1261g of Ethylene Oxide (EO), wherein the maximum pressure in the ethylene oxide introduction process is less than 1.4 MPa;
3) after the ethylene oxide is introduced, curing is carried out at the temperature of 151 ℃, and when the pressure is close to 1.12MPa in the curing process, nitrogen is introduced to keep the pressure at 1.15-1.25 MPa;
when the pressure in the reaction kettle is kept unchanged, the reaction is finished, and the whole curing time is about 1-2 h;
4) vacuumizing for 1.5-1h, cooling to 71-81 ℃, adding a neutralizing agent phosphoric acid to adjust the pH to 5-7, and obtaining modified liposome;
5) weighing modified liposome 95.2g, PEG411 monooleate 8g, vitamin E1.3 g, and Kathon solution 1.5 g. Mixing and stirring at 71 deg.C for 31min to obtain transparent modified liposome composition, and obtaining modified liposome mixture.
Modified liposome mixture preparation example 5:
in this example, the preparation of the modified liposome mixture comprises the following specific steps:
1) putting 911g of soybean oil containing 71 percent of phospholipid, 51.1g of cholesterol, 37.915g of glycerol, 1.995g of triethanolamine and 12g of KOH (catalyst) into an alkoxylation reaction kettle, and replacing nitrogen for three times; heating to 95-115 ℃ and dehydrating for 1 h;
2) then, heating to 121-151 ℃, introducing 1261g of Ethylene Oxide (EO), wherein the maximum pressure in the ethylene oxide introduction process is less than 1.4 MPa;
3) after the ethylene oxide is introduced, curing at the temperature of 121-151 ℃, and introducing nitrogen to keep the pressure at 1.15-1.25MPa when the pressure is close to 1.12MPa in the curing process;
when the pressure in the reaction kettle is kept unchanged, the reaction is finished, and the whole curing time is about 1-2 h;
4) vacuumizing for 1.5-1h, cooling to 71-81 ℃, adding a neutralizing agent phosphoric acid to adjust the pH to 5-7, and obtaining modified liposome;
5) 97.8g of modified liposomes were weighed out together with 2g of 11 polyglycerol monolaurate, 1.1g of vitamin C, 1.1g of kaempferol solution (11% strength). Mixing and stirring at 61 deg.C for 31min to obtain transparent modified liposome composition, and obtaining modified liposome mixture.
Adjuvant composition example 1
The components of the auxiliary composition in this example were as follows:
Figure BDA0003447566510000061
Figure BDA0003447566510000071
wherein the modified vegetable oil is an ethoxylated modified industrial soybean oil with the HLB value of 6.1 +/-1.5;
the modified liposome mixture is the product prepared in the modified liposome mixture preparation example 2;
the alcohol ether compound is diethylene glycol monobutyl ether;
the nonionic surfactant is C13 fatty alcohol polyoxyethylene ether, sorbitan and EO-PO block polyether;
the anionic surfactant is alpha-olefin sodium sulfonate.
The adjuvant composition in this example was prepared as follows:
(1) based on the ethoxylation modified industrial soybean oil with HLB value of 6.1 +/-1.5, 41.5g of the ethoxylation modified industrial soybean oil is accurately weighed, 11.1g of diethylene glycol monobutyl ether and 4.1g of C13 fatty alcohol polyoxyethylene ether are added, 2g of each of alpha-olefin sodium sulfonate and EO-PO block polyether surfactant are stirred and mixed uniformly to be used as an oil phase.
(2) 31g of deionized water is added into 5g of the modified liposome composition, and then 4g of each of fatty alcohol-polyoxyethylene ether and sorbitan surfactant of C13 are added to prepare aqueous phase mother liquor.
(3) Injecting the oil phase into the water phase mother liquor, complementing the oil phase to 111g with deionized water, mixing by adopting a high-speed shearing method, wherein the shearing speed is 15111r/min, the shearing time is 11-15 min, and mixing uniformly to obtain the synergistic composition, wherein the temperature needs to be controlled below 61 ℃ during mass preparation. Thus obtaining the ethoxylation modified soybean oil liposome synergistic composition 1A.
Adjuvant composition example 2
The components of the auxiliary composition in this example were as follows:
components Mass (g) g ═ parts
Modified vegetable oil 35.5
Modified liposome mixtures 6
Alcohol ether compound 4
Nonionic surfactant 17.5
Anionic surfactants 2
Deionized water --
Wherein the modified vegetable oil is ethoxylated modified rapeseed oil with HLB value of 5.1 +/-1.5;
the modified liposome mixture is the product prepared in the modified liposome mixture preparation example 3;
the alcohol ether compound is propylene glycol methyl ether acetate;
the nonionic surfactant is C6 fatty alcohol polyoxyethylene ether, C13 fatty alcohol polyoxyethylene ether, isomeric tridecanol polyoxyethylene ether and cocoyl diethanolamide;
the anionic surfactant is alpha-sulfo fatty acid methyl ester.
The adjuvant composition in this example was prepared as follows:
(1) 35.5g of ethoxylation modified rapeseed oil with the HLB value of 5.1 +/-1.5 is weighed, 4.1g of propylene glycol methyl ether acetate, 6.1g of C6 fatty alcohol-polyoxyethylene ether, 2.1g of alpha-sulfo fatty acid methyl ester and 4.1g of coco diethanolamide are added, and the mixture is stirred and mixed uniformly to form an oil phase.
(2) Taking 6.1g of the modified liposome and the composition, adding 35.1g of deionized water, 2.1g of ethylene glycol, 4.1g of C13 fatty alcohol polyoxyethylene ether and 3.5g of isomeric tridecanol surfactant, mixing and stirring uniformly to prepare aqueous phase mother liquor.
(3) Injecting the oil phase into the water phase mother liquor, complementing the oil phase to 111g with deionized water, mixing by adopting a high-speed shearing method, wherein the shearing speed is 11111r/min, the shearing time is 11-15 min, and uniformly mixing to obtain the synergistic composition, wherein the temperature needs to be controlled below 61 ℃ during mass preparation. Thus obtaining the ethoxylation modified rapeseed oil liposome synergistic composition 2A.
Adjuvant composition example 3
The components of the auxiliary composition in this example were as follows:
components Mass (g) g ═ parts
Modified vegetable oil 45
Modified liposome mixtures 11
Alcohol ether compound 11
Nonionic surfactant 11.5
Anionic surfactants 7.5
Deionized water --
Wherein the modified vegetable oil is ethoxylated modified soybean oil;
the modified liposome mixture is the product prepared in the modified liposome mixture preparation example 4;
the alcohol ether compound is dipropylene glycol butyl ether;
the nonionic surfactant is C9 fatty alcohol polyoxyethylene ether, sorbitan and EO-PO block polyether;
the anionic surfactant is oleoyloxy ethyl sodium sulfonate.
The adjuvant composition in this example was prepared as follows:
dipropylene glycol butyl ether 11.1g is adopted, C9 fatty alcohol-polyoxyethylene ether 2.1g is added, and the mixture is added into ethoxylation modified soybean oil 45.1g, and the mixture is stirred uniformly to complete emulsification. Sequentially adding 6.1g of sorbitan, 3.5g of EO-PO block polyether, 7.5g of oleoyloxy sodium ethanesulfonate and 4.1g of glycerol, adding 11.1g of modified liposome and composition in the stirring process, and supplementing to 111g by deionized water; thus obtaining the ethoxylation modified soybean oil liposome synergistic composition 3A.
Adjuvant composition example 4
The components of the auxiliary composition in this example were as follows:
components Mass (g) g ═ parts
Modified vegetable oil 45
Modified liposome mixtures 11
Alcohol ether compound 11
Nonionic surfactant 22
Anionic surfactants 2
Deionized water --
Wherein the modified vegetable oil is an ethylated modified palm oil;
the modified liposome mixture is the product prepared in the modified liposome mixture preparation example 5;
the alcohol ether compound is dipropylene glycol butyl ether;
the nonionic surfactant is C7 fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether phosphate, cocoyl diethanol acyl and EO-PO block polyether;
the anionic surfactant is alpha-olefin sodium sulfonate.
The adjuvant composition in this example was prepared as follows:
11.1g of propylene glycol monobutyl ether is adopted, 2.1g of C7 fatty alcohol-polyoxyethylene ether is added, and the mixture is added into 45.1g of ethyl modified palm oil and stirred uniformly. Then, 14.5g of cocoyl diethanolamide, 5.5g of alkylphenol polyoxyethylene ether phosphate, 2.1g of alpha-olefin sodium sulfonate and 2.1g of ethylene glycol are sequentially added, and in the stirring process, 8.1g of modified liposome and composition are added, and deionized water is used for supplementing to 111 g; thus obtaining the ethoxylation modified palm oil liposome synergistic composition 4A.
Pesticide synergist example 5
The pesticide synergist in the embodiment is an organosilicon product with MSDS number of 1144-1337-895-671, and the product is a commercial sample containing 75.1g of polyorganosiloxane and 25.1g of amorphous silicon and is marked as 5A.
Pesticide synergist example 6
The pesticide synergist in the embodiment is prepared by the following standard product numbers: the synergistic assistant product of Q/CY BHJ 1111-2115 is marked with synergistic components containing lecithin, vitamin E and the like and is marked as 6A.
Pesticide synergist example 7
The pesticide synergist in this example was 75% dioctyl sodium sulfosuccinate, and the solvent phase was water, which was designated as 7A.
Pesticide synergist example 8
The pesticide synergist in this embodiment is a commercially available methyl ester emulsion oil adjuvant, which contains 91% of methyl esterified vegetable oil and 11% of mixed anionic and nonionic emulsifiers, and is denoted as 8A.
Adjuvant composition comparative example 1
The processing mode in example 1 was changed to 311r/min of ordinary stirring, and the result is recorded as 1B.
Adjuvant composition comparative example 2
This example is essentially the same as example 3 except that conventional soybean oil was used instead of the ethoxylated modified soybean oil and the final product aid composition is designated 2B.
Adjuvant composition comparative example 3
The agricultural synergist in this comparative example, prepared in the following manner, was designated as 3B. Mixing and dissolving a sterol compound and a single-chain alkyl amphiphilic compound in a solvent, freeze-drying the mixture into powder, adding the powder into a buffer solution, and repeatedly freezing and thawing the powder to form a liposome dispersion liquid with a vesicle structure, wherein the method specifically comprises the following steps:
111mg of octadecylamine and 143.5mg of cholesterol were weighed out and dissolved in 6mL of benzene/methanol (5.4 mL of benzene, 1.6mL of methanol), and the solution was lyophilized overnight to remove the organic solvent. The mixture was hydrated by adding 21mL of MES-Tris buffer (pH 5.1). The reaction conditions comprise that liquid nitrogen is frozen for 1 minute, water bath at 71 ℃ is carried out for 11 minutes, the circulation is carried out for 5 times alternately, vortex oscillation is carried out for 31 seconds in successive circulation periods, the mixture is placed in an ultrasonic crusher to be treated for 21 minutes, 21 seconds are opened and 5 seconds of circulation is closed in the treatment periods, the amplitude is 41 percent, and the obtained agricultural synergist is obtained.
Adjuvant composition comparative example 4
The agricultural synergist in this comparative example, prepared in the following manner, was designated as 4B. The method specifically comprises the following steps:
adding 11% of lecithin, 21% of surfactant, 5-11% of oil auxiliary agent, 15-25% of polymer auxiliary agent, 1-5% of generated polymer compound, 5-11% of inorganic salt, 11-15% of wax and 15-31% of organic solvent into a reaction kettle in proportion, heating, stirring and mixing, wherein the stirring speed of the reaction kettle is 511-1111 rpm, the stirring temperature is 51-81 ℃, then homogenizing the mixed components under high pressure, and filtering, wherein the pressure of the homogenization is 21-31 MPa, so as to obtain the agricultural synergist.
Auxiliary composition comparative example 5
The agricultural synergist in this comparative example, prepared in the following manner, was denoted as 5B. Specifically, the method comprises the following steps:
weighing 35% of soybean lecithin (Chuangzhi engineering technology, llc, in Anqing), 5% of D-limonene (zhong new material, llc, Jiangxi), 20% of Lutensol TO2 (branched-chain fatty alcohol-polyoxyethylene ether, BASF), 25% of propionic acid (Jinan, ao Chen chemical engineering, inc), and deionized water TO make up TO 100%. The agricultural synergist can be obtained by mixing and stirring the raw materials until the raw materials are transparent and uniform and filtering the mixture.
Adjuvant composition comparative example 6
The processing mode in example 1 was changed to ordinary stirring at 5111r/min, and the result was recorded as 6B.
Adjuvant composition comparative example 7
This embodiment is basically the same as embodiment 1 except that: unmodified liposomes of 30% phospholipid soybean oil and cholesterol were used.
Performance verification experiment 1
According to the method of the stem and leaf spraying method (NY/T1155.4-2116) of the 4 th part of herbicide part, which conforms to the indoor bioassay test criteria of pesticides, a sampling test is carried out, targets are collected from paddy fields near the Yizheng city, the amount of cyhalofop-butyl is increased from 51g per mu of the conventional dosage to 211g, the better control effect cannot be achieved, the resistance is very serious, and the resistance is up to 121 times as high as that of a sensitive strain (the birth control center of the chemical research institute in Zhejiang province) in indoor bioassay;
target: the weed targets selected by the project are all planted with resistance weed seeds collected in the field, namely moleplant seed and barnyard grass;
medicament: the auxiliary agent compositions 1A to 4A or the pesticide synergist 5A to 8A or the compositions 1B to 5B are diluted according to the dilution times shown in the table 2 and are prepared into a tank-mixed liquid medicine together with 11 percent cyhalofop-butyl emulsifiable concentrate herbicide;
spraying mode: manually spraying (instead of flying prevention operation, so that the influence of liquid medicine drifting can be avoided) on the corresponding target weeds, and observing the respective growth conditions of crops and weeds;
the test results are shown in table 1 below.
TABLE 1 test results of examples and comparative examples
Figure BDA0003447566510000111
Note: in the table, the degree of difference of the significance marks of the Duncan's new repolarization method is represented by an alphabetical sequence according to the LSD minimum significant difference method; wherein a, b, c, d, e, f represent significant differences between any two values; in addition, ab has no significant difference from a or b or bc, bc has no significant difference from b or c or ab or cd, cd has no significant difference from d or c or bc or de, de has no significant difference from d or e or cd or de or cde, and cde has no significant difference from d or c or e or bc or de or cd.
As can be seen from the above table:
the auxiliary agent composition 1A-4A provided by the invention has excellent synergistic degree;
compared with the commercially available pesticide synergist 5A-8A, the assistant composition 1A-4A still has remarkable advantages, particularly 1A;
taking the auxiliary composition 1A provided by the present invention as an example, compared with the comparative auxiliary compositions 1B and 6B, the effect of the auxiliary composition can be ensured only if the shear rate achieved in the preparation process needs to reach a certain level.
The comparative auxiliary composition 2B is prepared from a common soybean oil instead of a modified vegetable oil (ethoxylated modified soybean oil), and the auxiliary composition 1A provided by the invention has a significant synergistic advantage compared with the comparative auxiliary composition 2B.
The auxiliary composition 7B used as a comparison is prepared by using a non-modified liposome instead of a modified liposome as a raw material, and taking the auxiliary composition 1A provided by the invention as an example, the auxiliary composition has a significant synergistic advantage compared with the auxiliary composition 2B used as a comparison.
The auxiliary composition 5B used as a comparison is prepared from a non-modified liposome as a raw material, and taking the auxiliary composition 1A provided by the invention as an example, the auxiliary composition has a significant synergistic advantage compared with the auxiliary composition 2B used as a comparison.
In addition, the comparative adjuvant compositions 1B-6B have a limited synergistic effect, although a certain synergistic effect is obtained.
Performance verification experiment 2
The pesticide receiving amount of crops, targets (insects, diseases, grass) and the like in unit area is improved, the liquid medicine fog drops are prevented from drifting and are transferred to non-target areas along with air flow, and the pesticide receiving amount is one of the bases for ensuring pesticide effect. The key point is the particle size of the fog drops, and the particle size range of the fog drops of 151-311 mu m is generally considered by the plant protection community as the optimal biological particle size range in the application scene of the air defense. The larger the droplet size is in this range, the less the flying spray drifts, the higher the deposition amount, and the more excellent control effect can be obtained. The advantages of low-volume spraying in the flying defense operation can be reserved, and the problem of liquid medicine drifting in the flying defense operation process can be effectively solved.
The instrument comprises the following steps: spraying under the conditions of determined nozzle model and pressure by adopting a device for detecting the performance parameters of pesticide droplets treated by a flying prevention auxiliary agent (CN211118672U) of the company according to the method of the patent, and testing the particle size data DV1, DV5 and DV9 of the sprayed droplets;
medicament: the auxiliary agent compositions 1A to 4A or the pesticide synergist 5A to 8A or the compositions 1B to 5B are diluted according to the dilution times shown in the table 2 and are prepared into a tank-mixed liquid medicine together with 11 percent cyhalofop-butyl emulsifiable concentrate herbicide;
synchronously calculating to obtain the particle size distribution span, wherein the calculation formula is as follows:
span (DV9-DV1)/DV 5;
the particle size span can reflect the uniformity of particle size distribution, and the numerical value is closer to 1, which means that the droplet spectrum distribution is more normal and the droplets are more uniform. Specifically, as shown in table 2 below.
TABLE 2 summary of droplet size distribution data
Figure BDA0003447566510000121
Figure BDA0003447566510000131
As can be seen from the table data, under the same spraying condition, the auxiliary agents described in examples 1A-4A can enable the particle size spectrum of the fog drops to fall into the range of the optimal biological particle size (150-300 μm) more, and the particle size spectrum span is smaller, so that the spraying agent is remarkably superior to other examples and comparative examples. The auxiliary agent is used in a flying prevention scene, so that the particle size spectrum of flying spray-proof droplets can be effectively adjusted, the pesticide application process can be more effectively resistant to drifting, the deposition and detention of liquid medicine droplets on the surface of a target are promoted, and the liquid medicine is promoted to exert pesticide effect.
Performance verification experiment 3
In order to more clearly and specifically describe the effect of the pesticide synergist composition provided by the embodiment of the present invention after being mixed with herbicides, the adjuvant composition 1A is taken as an example and is respectively compounded with different herbicides, specifically:
a first group: indoor bioassay test for preventing and controlling grassy weeds in paddy fields by using 11% cyhalofop-butyl emulsifiable concentrate, planting barnyard grass and moleplant seeds in a flowerpot with the diameter of 9cm in advance, carrying out spraying prevention and control when weeds are in a 3-leaf stage, uniformly spraying by using a 3WP-2111 type walking spraying tower as spraying equipment, and carrying out result investigation 21 days after the pesticide is applied, wherein the result shows that the pesticide effect is improved by 26.93% compared with that without adding a synergist after the synergist is added to the moleplant seeds, and the pesticide effect is improved by 26.28% compared with that without adding the synergist after the barnyard grass is added, so that the effect is obvious in synergistic effect on the 11% cyhalofop-butyl emulsifiable concentrate after the synergist is added in a tank mixing manner.
Second group: indoor bioassay test for preventing and treating gramineous weeds in wheat fields by using 5% pinoxaden emulsifiable solution comprises the steps of planting bluegrass and alopecurus aegypti in a flowerpot with the diameter of 9cm in advance, carrying out spraying prevention and treatment when weeds are about 2-3 leaf stages, uniformly spraying by using a 3WP-2111 type walking spraying tower as spraying equipment, and carrying out result investigation 21 days after application, wherein the result shows that the pesticide effect is improved by 23.37% when synergist is added to the bluegrass and is improved by 15.19% when the synergist is added to the alopecurus aegypti.
Third group: indoor bioassay test for preventing and treating gramineous weeds in rice fields by 25g/L penoxsulam oil suspension agent comprises the steps of planting moleplant seeds and barnyard grass in a flowerpot with the diameter of 9cm in advance, carrying out spraying prevention and treatment when weeds are about 2-3 leaf stages, uniformly spraying by adopting a 3WP-2111 type walking spraying tower as spraying equipment, and carrying out result investigation 21 days after the application of the penoxsulam oil suspension agent, wherein the effect ratio is improved by 18.64% after the synergist is added to the moleplant seeds, and the effect ratio is improved by 14.18% after the synergist is added to the barnyard grass, so that the penoxsulam oil suspension agent has an obvious synergistic effect on 25g/L penoxsulam oil suspension agent after the synergist is added in a tank mixing manner.
And a fourth group: indoor bioassay test for preventing and treating uncultivated land weeds by using 211g/L glufosinate-ammonium aqua comprises the steps of planting barnyard grass and amaranthus retroflexus in a flowerpot with the diameter of 9cm in advance, carrying out spraying prevention and treatment when the weeds are in a 3-4 leaf stage, uniformly spraying by adopting a 3WP-2111 type walking spray tower as spraying equipment, and carrying out result investigation 21 days after the application of the glufosinate-ammonium aqua, wherein the effect is improved by 16.47% compared with that after a synergist is added to the barnyard grass, and the effect is improved by 15.13% compared with that after the synergist is added to the amaranthus retroflexus, so that the indoor bioassay test has an obvious synergistic effect on the 211g/L glufosinate-ammonium aqua after the synergist is added in a tank mixing manner.
And a fifth group: according to indoor bioassay tests for controlling uncultivated land weeds (311ml) by using the 31% glyphosate isopropylamine aqua, barnyard grass and amaranthus retroflexus are planted in a flowerpot with the diameter of 9cm in advance, spraying control is carried out when the weeds are in about 3-4 leaf stage, spraying equipment adopts a 3WP-2111 type walking spraying tower to carry out uniform spraying, and result investigation is carried out 21 days after the application of the glyphosate isopropylamine aqua.
A sixth group: in an indoor test for controlling annual gramineous weeds (75ml) in rice fields by 21% of cyhalofop-butyl-metamifop emulsifiable concentrate, a 9 cm-diameter flowerpot is used for planting moleplant seeds and barnyard grass in advance, spraying control is carried out when weeds are about 2-3 leaf stages, a 3WP-2111 type walking spray tower is adopted as spraying equipment, spraying is carried out uniformly, and result investigation is carried out 21 days after the application of the herbicide, so that the effect is improved by 13.17% compared with that after the synergist is added to the moleplant seeds, and the effect is improved by 16.64% compared with that after the synergist is added to the barnyard grass, and therefore, after the synergist is added in a tank mixing manner, the herbicide has an obvious synergistic effect on 25g/L penoxsulam oil suspension.
A seventh group: indoor bioassay test (211ml) for controlling weeds in corn fields by using 24% nicotiana atrazine-tare dispersible oil suspending agent, planting Amaranthus retroflexus and Echinochloa crusgalli in a flowerpot with the diameter of 9cm in advance, carrying out spraying control when weeds are at about 2-3 leaf stage, uniformly spraying by using a 3WP-2111 type walking spraying tower as spraying equipment, and carrying out result investigation 21 days after the application of the suspending agent to obtain the result, wherein the effect is improved by 15.51% compared with that of the suspending agent which is not added after the synergist is added to the Echinochloa crusgallium crudus, and the effect is improved by 14.92% compared with that of the suspending agent which is not added after the synergist is added to the Amaranthus retroflexus, so that the indoor bioassay test has a better synergistic effect on 211g/L of glufosinate solution after the synergist is added in a tank mixing manner.
The effects of the above groups are shown in table 3 below.
TABLE 3 series of herbicide raw test results
Figure BDA0003447566510000141
Figure BDA0003447566510000151
Note: in the table "-" indicates that the target is not the main prevention object of the reagent and the corresponding test is not carried out;
in the table, the degree of difference of the significance marks of the Duncan's new repolarization method is represented by an alphabetical sequence according to the LSD minimum significant difference method; wherein a, b, c, d, e, f, g, h, represent any significant difference between any two values; in addition, ab does not have a significant difference from a or b or bc, bc does not have a significant difference from b or c or cd, cd does not have a significant difference from d or c or bc or de, and de does not have a significant difference from d or e or cd.
Performance verification experiment 4
Meanwhile, in a performance verification experiment 3, when a first group (11% of cyhalofop-butyl emulsifiable concentrate and 11% of cyhalofop-butyl emulsifiable concentrate are mixed with the synergistic composition of the invention) is researched, it is found that compared with the situation that only 11% of cyhalofop-butyl emulsifiable concentrate is used for preventing and controlling gramineous weeds in a paddy field (japonica rice-south japonica 5155), the effect of improving the control effect of resistant weeds (the pesticide effect on stephania japonica is improved by 26.93%, and the pesticide effect on barnyard grass is improved by 26.28%) is achieved by using the liquid medicine obtained by mixing 11% of cyhalofop-butyl emulsifiable concentrate and the synergistic composition of the invention for preventing and controlling gramineous weeds in the paddy field (japonica rice-south japonica 5155).
Meanwhile, after the pesticide liquid obtained by mixing 11% of cyhalofop-butyl missible oil with the synergistic composition is applied to a paddy field (japonica rice-Nanjing 5155), the absorption and metabolism of various nutrient elements in soil by crops are remarkably improved, the synergistic effect of weeding is intuitively shown, meanwhile, the vegetative growth of the crops is remarkably promoted, the leaf color is dark green, the chlorophyll content is improved, and the thousand-grain weight is increased. The paddy field to which only 11% cyhalofop-butyl emulsifiable concentrate was applied did not have this effect.
Furthermore, according to the method of the agricultural industry standard of the people's republic of China-determination of chlorophyll content in fruits, vegetables and products thereof (spectrophotometry) NY/T3182-2117, sampling investigation was carried out, and flag leaves of rice in each treatment block were randomly cut out to measure the chlorophyll content, as shown in the following Table 4.
TABLE 4 chlorophyll test results
Figure BDA0003447566510000152
The detection data show that the chlorophyll content of the rice flag leaves is remarkably improved by adding a group of treatment of weeding by the synergistic additive, and the yield investigation when the rice is harvested is further prolonged to find that the average thousand-grain weight of the treated rice is remarkably higher than that of the group without adding the adjuvant composition of the invention, which indicates that the improvement of the chlorophyll content of the rice flag leaves and the average thousand-grain weight of the rice is not the effect of the herbicide cyhalofop-butyl; the reason is that the auxiliary composition provided by the invention promotes the absorption and transmission of the herbicide in the weed body, promotes the absorption and transmission of mineral elements of crops, increases the accumulation of nutrients of the crops and promotes the yield.
In addition, the comparative adjuvant compositions 1B-6B, agreed not to have the effect of increasing the average thousand kernel weight of rice with a chlorophyll content in flag leaves of rice.
More specifically, although exemplary embodiments of the invention have been described herein, the invention is not limited to these embodiments, but includes any and all embodiments modified, omitted, combined, e.g., between various embodiments, adapted and/or substituted, as would be recognized by those skilled in the art from the foregoing detailed description. The limitations in the claims are to be interpreted broadly based the language employed in the claims and not limited to examples described in the foregoing detailed description or during the prosecution of the application, which examples are to be construed as non-exclusive. Any steps recited in any method or process claims may be executed in any order and are not limited to the order presented in the claims. The scope of the invention should, therefore, be determined only by the appended claims and their legal equivalents, rather than by the descriptions and examples given above.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control. When a mass, concentration, temperature, time, or other value or parameter is expressed as a range, preferred range, or as a range of values bounded by a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, a range of 1 to 51 should be understood to include any number, combination of numbers, or subrange selected from 1, 2, 3, 4, 5, 6, 7, 8, 9, 11, 12, 13, 14, 15, 16, 17, 18, 19, 21, 22, 23, 24, 25, 26, 27, 28, 29, 31, 32, 33, 34, 35, 36, 37, 38, 39, 41, 42, 43, 44, 45, 46, 47, 48, 49, or 51, and all fractional values between the above integers, e.g., 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, and 1.9. With respect to sub-ranges, specifically consider "nested sub-ranges" that extend from any endpoint within the range. For example, nested sub-ranges of exemplary ranges 1-51 may include 1-11, 1-21, 1-31, and 1-41 in one direction, or 51-41, 51-31, 51-21, and 51-11 in another direction.

Claims (10)

1. An auxiliary composition for improving the effect of agricultural drugs, which is characterized in that: comprises the following components in parts by weight:
Figure FDA0003447566500000011
2. the adjuvant composition for improving the effect of agricultural drugs according to claim 1, wherein: the modified vegetable oil is one or a combination of more of methyl esterification modified vegetable oil, ethoxylation modified vegetable oil and epoxidation modified vegetable oil.
3. The adjuvant composition for improving the effect of agricultural drugs according to claim 1, wherein: the vegetable oil comprises one or more of soybean oil, rapeseed oil, palm oil, olive oil, coconut oil, orange peel oil, citronella oil and turpentine oil.
4. The adjuvant composition for improving the effect of agricultural drugs according to claim 1, wherein: the alcohol ether compound is one or more of ethylene glycol, propylene glycol, diethylene glycol monobutyl ether, ethylene glycol butyl ether, propylene glycol methyl ether, diethylene glycol ethyl ether, ethylene glycol phenyl ether, ethylene glycol hexyl ether, diethylene glycol hexyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether, tripropylene glycol methyl ether, propylene glycol methyl ether acetate, propylene glycol propyl ether, dipropylene glycol propyl ether, propylene glycol butyl ether, dipropylene glycol butyl ether, tripropylene glycol butyl ether, propylene glycol phenyl ether and n-propyl propionate.
5. The adjuvant composition for improving the effect of agricultural drugs according to claim 1, wherein: the nonionic surfactant is one or more of polyoxyethylene type nonionic surfactant, polyalcohol type nonionic surfactant, alkanolamide type nonionic surfactant, polyether type nonionic surfactant and amine oxide type nonionic surfactant.
6. The adjuvant composition for improving the effect of agricultural drugs according to claim 1, wherein: the anionic surfactant is one or a combination of more of alpha-olefin sodium sulfonate, alpha-sulfo fatty acid methyl ester, oleoyloxy ethyl sodium sulfonate, N-oleoyl N-methyl sodium taurate and diisooctyl succinate sodium sulfonate.
7. An adjuvant composition for enhancing the effectiveness of an agricultural drug according to any one of claims 1 to 6, wherein: the modified liposome is prepared by the following method:
1) modification of liposomes: heating and dehydrating the mixture of glycerophospholipid, sterol and polyhydroxy compound by using a catalyst; the temperature rise is 95-105 ℃, and the dehydration treatment time is 1-3 h;
2) then, heating to 120-150 ℃, and introducing ethylene oxide, wherein the maximum pressure is controlled to be not more than 0.4MPa in the ethylene oxide introducing process;
3) after the ethylene oxide is introduced, reacting at the temperature of 120-150 ℃ until the pressure is not changed, and finishing the reaction;
before the reaction is finished, the pressure needs to be controlled to be 0.02-0.25 MPa;
4) cooling (70-80 deg.C), adding neutralizing agent to adjust pH to 5-7;
5) respectively weighing the modified liposome, the fatty acid ester substances, the vitamins and the kasong solution, and mixing and stirring at 60-70 ℃ to obtain a modified liposome mixture;
the modified liposome accounts for 89.2-97.8 wt%, the fatty acid ester substances account for 2-10 wt%, the vitamins account for 0.1-0.5 wt%, and the 10% cason aqueous solution accounts for 0.1-0.3 wt%.
8. The adjuvant composition for improving the effect of agricultural drugs according to claim 7, wherein: the fatty acid ester substance is one or more of trimethylolpropane fatty acid ester, propylene glycol fatty acid ester, pentaerythritol fatty acid ester, polyethylene glycol fatty acid monoester, polyethylene glycol fatty acid diester, fatty acid polyoxyethylene ether fatty acid ester, polyglycerol fatty acid ester, sorbitan fatty acid and sucrose fatty acid ester;
the polyhydroxy compound is a composition of alcohol and alcohol amine, and the alcohol is one or two of glycerol and glycol; the alcohol amine is one or two of diethanolamine and triethanolamine; the mass ratio of the alcohols is 55-95%, and the mass ratio of the alcohol amine is 5-45%;
the glycerol phosphatide is one or a combination of more of soybean phosphatide, phosphatidic acid, sunflower phosphatide, rapeseed phosphatide, canola phosphatide, linseed phosphatide, castor oil phosphatide, soybean phosphatide hydrogenated derivative, phosphatidic acid hydrogenated derivative, sunflower phosphatide hydrogenated derivative, rapeseed phosphatide hydrogenated derivative, canola phosphatide hydrogenated derivative, linseed phosphatide hydrogenated derivative and castor oil phosphatide hydrogenated derivative;
the catalyst is one or a combination of more of sodium methoxide, potassium methoxide, sodium hydroxide and potassium hydroxide; the sterol is one or more of beta-sitosterol, beta-sitostanol, stigmasterol, stigmastanol, campesterol, campestanol, ergosterol, avenasterol, brassicasterol and cholesterol.
9. A process for the preparation of an adjuvant composition for improving the effectiveness of an agricultural drug according to any one of claims 1 to 8, wherein: the method comprises the following steps:
oil phase preparation: contacting and mixing the modified vegetable oil and the alcohol ether solvent, and then adding an anionic surfactant and a nonionic surfactant for contacting and mixing;
aqueous phase (mother liquor) configuration: contacting and mixing the modified liposome mixture with a nonionic surfactant;
injecting the oil phase into the water phase, and carrying out shearing treatment to obtain the synergistic composition; the shearing speed is 10000-20000 r/min, and the shearing time is 10-15 min.
10. The method for preparing an adjuvant composition for improving agricultural effects according to claim 9, wherein:
the mass ratio of the nonionic surface active agent in the oil phase preparation process to the nonionic surface active agent in the water phase (mother liquor) preparation process is (1-3): (2-5).
CN202111661527.5A 2021-12-30 2021-12-30 Auxiliary composition for improving agricultural drug effect and preparation method thereof Pending CN114365743A (en)

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CN109258634A (en) * 2018-11-08 2019-01-25 江西普菲迅抗性杂草防治有限公司 A kind of pesticide synergistic volume increase auxiliary agent and preparation method thereof
CN109644998A (en) * 2018-12-26 2019-04-19 中化化工科学技术研究总院有限公司 One kind flying anti-auxiliary agent and the preparation method and application thereof
CN110583641A (en) * 2019-09-05 2019-12-20 新疆农业科学院核技术生物技术研究所（新疆维吾尔自治区生物技术研究中心） Agricultural auxiliary agent for flight control, and preparation method and application thereof
CN110742064A (en) * 2019-11-05 2020-02-04 江苏擎宇化工科技有限公司 Modified liposome and composition, preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102781232A (en) * 2010-03-01 2012-11-14 日本化药株式会社 Pest controlling composition
CN106689122A (en) * 2016-12-12 2017-05-24 北京广源益农化学有限责任公司 Spray aid for agricultural aviation plant protection spray or ultra-low-capacity spray and application
CN109258634A (en) * 2018-11-08 2019-01-25 江西普菲迅抗性杂草防治有限公司 A kind of pesticide synergistic volume increase auxiliary agent and preparation method thereof
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