CN113796374A - Pesticide containing neem oil special for flight control and preparation method thereof - Google Patents

Pesticide containing neem oil special for flight control and preparation method thereof Download PDF

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Publication number
CN113796374A
CN113796374A CN202111124430.0A CN202111124430A CN113796374A CN 113796374 A CN113796374 A CN 113796374A CN 202111124430 A CN202111124430 A CN 202111124430A CN 113796374 A CN113796374 A CN 113796374A
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neem oil
pesticide
polyoxyethylene
oil
antioxidant
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CN113796374B (en
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黄素青
张志祥
徐汉虹
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South China Agricultural University
Zhongkai University of Agriculture and Engineering
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South China Agricultural University
Zhongkai University of Agriculture and Engineering
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    • AHUMAN NECESSITIES
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    • 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
    • A01N25/02Biocides, 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
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • A01N25/06Aerosols
    • AHUMAN NECESSITIES
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    • A01N37/36Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
    • A01N37/38Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
    • A01N37/40Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic ring system
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    • 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
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    • A01N47/28Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/34Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the groups, e.g. biuret; Thio analogues thereof; Urea-aldehyde condensation products
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    • A01N47/28Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/38Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
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    • A01N47/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/40Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
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    • A01N51/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
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    • A01N65/08Magnoliopsida [dicotyledons]
    • A01N65/26Meliaceae [Chinaberry or Mahogany family], e.g. mahogany, langsat or neem
    • 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
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Abstract

The invention discloses a pesticide containing neem oil special for flight control, which comprises the following components in percentage by weight: 0.2-40% of pesticide active agent, 10-25% of surfactant, 5-20% of cosolvent, 0.05-1% of antioxidant and the balance of neem oil. Compared with the prior art, the special pesticide for the flight control has obvious anti-drift effect and obvious field pesticide effect.

Description

Pesticide containing neem oil special for flight control and preparation method thereof
Technical Field
The invention relates to the technical field of plant protection, in particular to a pesticide containing neem oil special for flight control and a preparation method thereof.
Background
The flying prevention plant protection is a newly-developed thing which develops rapidly, China has 4 tens of thousands of agricultural unmanned aerial vehicles in 2018, the farmland area of the agricultural unmanned aerial vehicles for pest control exceeds 1 hundred million mu, the operation area is 2.6 hundred million mu times, and pesticide flying prevention becomes a great trend. However, apart from the lack of special chemicals suitable for flight control, another problem is that large-area spraying is adopted during flight control, and the plant protection is indiscriminately hit against pests, natural enemies, bees and other organisms, which is contrary to the plant protection policy of comprehensive agricultural control. On the other hand, different from the traditional spraying mode, the flying prevention agent is sprayed at high concentration, only 500 ml of water is used for each mu of land, the dilution ratio is only 30-50 times, the concentration of the drug is high, and the drug injury is easy to generate, especially in tender places such as leaf tips, leaf edges and the like. Furthermore, the flying prevention agent used in China at present is developed and used based on a manual backpack sprayer, the using requirements of the flying prevention agent are not met, flocculation, deposition and precipitation can occur in the flying prevention process, the pesticide effect is reduced, a spray head is blocked, the pesticide damage is caused, and the field control effect is poor.
Thus, there is a need for suitable dosage forms of flight control agents.
Disclosure of Invention
The invention aims to solve the problems of flocculation, deposition and precipitation, nozzle blockage, pesticide effect reduction and poor field control effect caused by pesticide damage in the using process of the flight control pesticide in the prior art, and provides a special pesticide containing neem oil for flight control, wherein the physical properties of the pesticide liquid of the special pesticide for flight control are different from those of the existing flight control pesticide, so that the pesticide liquid can inhibit evaporation of pesticide drops sprayed out of a sprayer, prolong the drying time of the pesticide drops, reduce the formation of tiny pesticide drops, form larger pesticide drops, accelerate the settlement of the pesticide liquid, have obvious anti-drift effect and have obvious field pesticide effect.
In order to achieve the purpose, the invention adopts the following technical scheme:
a pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight: 0.2-40% of pesticide active agent, 10-25% of surfactant, 5-20% of cosolvent, 0.05-1% of antioxidant and the balance of neem oil.
The neem oil is a downstream product from the production process of biological pesticide nimbin, and is vegetable oil obtained by mechanically cold-pressing neem kernels, which has a repellent effect on various pests, and can be used as a pesticide auxiliary agent to reduce the drug resistance, increase the drug effect, prevent various pests and fungal diseases and protect grains from mold infection. As a natural plant extract, the plant extract is safe and environment-friendly and has no pollution. Neem oil is also a natural oil, and the oil contains a large amount of oleic acid and fatty acid, and the oleic acid has affinity with the oil on the surface of a target, so that liquid drops can be quickly attached to and spread on the target. The fatty acid forms a molecular film on the surface of the droplet, thereby reducing the volatilization of water. The main active component in neem oil is Salannin analogue, and has strong repellent activity and feeding deterrent activity on locusta migratoria, red round scale, cucumber striped beetle, housefly and Japanese beetle. Through reasonable blending, the insecticidal composition can show synergistic effect with insecticidal active ingredients such as chlorantraniliprole, emamectin benzoate, cyantraniliprole, tetrachlorantraniliprole, high-efficiency cypermethrin, lufenuron, methoxyfenozide, indoxacarb, imidacloprid, chlorfenapyr, flubendiamide, spinetoram, nitenpyram, chlorpyrifos, hexaflumuron, sulfoxaflor, acetamiprid and the like.
Furthermore, the pesticide special for flying prevention and containing neem oil further comprises 0.001-5 wt% of an antifreeze agent, wherein the antifreeze agent comprises one or more of glycerol, propylene glycol and urea.
Further, the pesticide active agent comprises one or more of chlorantraniliprole, emamectin benzoate, cyantraniliprole, tetrachlorantraniliprole, beta-cypermethrin, lufenuron, methoxyfenozide, indoxacarb, imidacloprid, chlorfenapyr, flubendiamide, spinetoram, nitenpyram, chlorpyrifos, hexaflumuron, sulfoxaflor and acetamiprid.
Further, the surfactant includes one or a mixture of two or more of silicone polyoxyethylene ether, fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, castor oil ethylene oxide derivative, castor oil propylene oxide derivative, alkylphenol polyoxyethylene polyoxypropylene ether, a chimeric of alkylphenol polyoxyethylene and polyoxypropylene ether, an alkylphenol polyoxyethylene formaldehyde condensate, an alkyldiphenolpolyoxyethylene polyoxypropylene ether, a chimeric of alkyldiphenolpolyoxyethylene and polyoxypropylene ether, an alkyldiphenolpolyoxyethylene formaldehyde condensate, an alkylnaphthalene polyoxyethylene polyoxypropylene ether, a chimeric of alkylnaphthalene polyoxyethylene and polyoxypropylene ether, or an alkylnaphthalene polyoxyethylene formaldehyde condensate.
Furthermore, the cosolvent comprises one or a mixture of more than two of ethylene glycol diacetate, ethylene glycol, isopropanol and methyl oleate.
Further, the antioxidant comprises one or more of propyl gallate, butyl hydroxy anisol, dibutyl hydroxy toluene and tert-butyl hydroquinone.
The invention also provides a preparation method of the pesticide containing neem oil special for flight control, which comprises the following steps:
s1, adding heat conducting oil into the reaction kettle and heating to dry the interior of the reaction kettle;
s2, adding a cosolvent into a dry and anhydrous reaction kettle, then adding a pesticide active agent, and stirring at the rotating speed of 1000-1500r/min for 10-20 min;
s3, adding a surfactant into the reaction kettle, and continuously stirring for 10-15 min;
s4, adding neem oil into the reaction kettle, and continuously stirring for 10-15 min;
s5, adding an antioxidant into the reaction kettle, and continuously stirring for 5-10 min;
s6, adding an antifreeze agent into the reaction kettle, and continuously stirring for 5-10 min;
and S7, naturally cooling to room temperature after stirring.
Compared with the prior art, the invention has the beneficial effects that:
1. by reasonably adjusting the proportion of the neem oil and the pesticide active agent, the generation of tiny fogdrops is reduced, the evaporation of the fogdrops is inhibited, the drying time of the fogdrops is prolonged, the liquid medicine sedimentation is accelerated, the distribution range of a fogdrops spectrum is changed, and the neem oil and the pesticide active agent have better performances of transpiration resistance, drift resistance, wetting, adhesion, synergy and the like.
2. The pesticide containing neem oil specially used for flying prevention has synergistic effect on rice planthopper, aphid, diamond back moth and spodoptera frugiperda, further reduces the dosage of chemical pesticide, and has important significance on pollution-free production of crops.
3. The pesticide containing neem oil specially used for flying prevention has strong repellent activity and food refusal activity to locusta migratoria, red round scale, cucumber striped beetle, housefly, Japanese beetle and the like.
Drawings
FIG. 1 is a graph showing the results of the field efficacy test of the pesticide for plant protection containing neem oil on cabbage caterpillar according to example 1;
FIG. 2 is a graph showing the results of the field efficacy test of the Neem oil-containing flying control pesticide of example 3 of the present invention against Spodoptera frugiperda;
FIG. 3 is a graph showing the results of the field efficacy test of the pesticide for plant protection containing Neem oil according to example 14 against rice planthopper;
FIG. 4 is a graph showing the results of the field efficacy test of the pesticide for plant protection containing Neem oil on Aphis gossypii Glover according to example 8 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of the present invention.
Example 1
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
4.5% of pesticide active agent, 10% of surfactant, 10% of cosolvent, 0.5% of antioxidant, 5% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agent is beta-cypermethrin.
In this embodiment, the surfactant is castor oil polyoxyethylene ether.
In this embodiment, the co-solvent is ethylene glycol diacetate.
In this embodiment, the antioxidant is butylated hydroxyanisole.
In this embodiment, the antifreeze agent is glycerol.
A preparation method of a pesticide containing neem oil special for flight control comprises the following steps:
s1, heating the heat conduction oil in the reaction kettle for drying, so that the interior of the container is dry and anhydrous;
s2, adding the cosolvent into an anhydrous container, then adding the active substance, and stirring for 10-20min by using an electric stirrer at 1500 r/min;
s3, adding a surfactant, and continuously stirring for 10-15 min;
s4, adding neem oil, and continuing stirring for 10-15 min;
s5, adding an antioxidant, and continuously stirring for 5-10 min;
s6, adding an antifreeze agent and continuously stirring for 5-10 min;
and S7, naturally cooling to room temperature after stirring.
Example 2
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
10% of pesticide active agent, 18% of surfactant, 15% of cosolvent, 0.1% of antioxidant, 4% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agent is cyantraniliprole.
In this embodiment, the surfactant is alkylphenol ethoxylates.
In this embodiment, the co-solvent is methyl oleate.
In this embodiment, the antioxidant is dibutylhydroxytoluene.
In this embodiment, the antifreeze agent is propylene glycol.
The preparation method refers to the preparation process of example 1.
Example 3
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
10% of pesticide active agent, 12% of surfactant, 14% of cosolvent, 0.15% of antioxidant, 3% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agent is chlorfenapyr.
In this embodiment, the surfactant is an alkylphenol ethoxylate phosphate.
In this embodiment, the co-solvent is ethylene glycol diacetate.
In this embodiment, the antioxidant is butylated hydroxyanisole.
In this embodiment, the antifreeze agent is urea.
The preparation method refers to the preparation process of example 1.
Example 4
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
20% of pesticide active agent, 15% of surfactant, 13% of cosolvent, 0.1% of antioxidant, 5% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agent is indoxacarb.
In this embodiment, the surfactant is a phenylethylphenol polyoxyethylene ether phosphate.
In this embodiment, the co-solvent is isopropanol.
In this embodiment, the antioxidant is tertiary butyl hydroquinone.
In this embodiment, the antifreeze agent is propylene glycol.
The preparation method refers to the preparation process of example 1.
Example 5
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
5% of pesticide active agent, 11% of surfactant, 12% of cosolvent, 0.05% of antioxidant, 4% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agent is a mixture of emamectin benzoate and lufenuron, and the mass ratio of the emamectin benzoate to the lufenuron is 1: 4.
in this embodiment, the surfactant is fatty alcohol-polyoxyethylene ether sodium sulfate and phenethyl phenol polyoxyethylene ether, and the mass ratio of the fatty alcohol-polyoxyethylene ether sodium sulfate to the phenethyl phenol polyoxyethylene ether is 7: 4.
in this embodiment, the co-solvent is glycerol.
In this embodiment, the antioxidant is propyl gallate.
In this embodiment, the antifreeze agent is urea.
The preparation method refers to the preparation process of example 1.
Example 6
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
25% of pesticide active agent, 20% of surfactant, 9% of cosolvent, 0.1% of antioxidant, 3% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agents are chlorantraniliprole and acetamiprid, and the mass ratio of the chlorantraniliprole to the acetamiprid is 2: 3.
in this embodiment, the surfactant is lauryl diethanolamine and sodium fatty alcohol-polyoxyethylene ether sulfate, and the mass ratio of lauryl diethanolamine to sodium fatty alcohol-polyoxyethylene ether sulfate is 1: 1.
in this embodiment, the cosolvent is ethanol and methyl oleate, and the mass ratio of ethanol to methyl oleate is 1: 2.
in this embodiment, the antioxidant is propyl gallate.
In this embodiment, the antifreeze agent is glycerol.
The preparation method refers to the preparation process of example 1.
Example 7
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
5% of pesticide active agent, 10% of surfactant, 8% of cosolvent, 0.2% of antioxidant, 4% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticidal active agent is lufenuron.
In this embodiment, the surfactant is fatty alcohol polyoxyethylene ether phosphate.
In this embodiment, the co-solvent is methyl oleate.
In this embodiment, the antioxidant is tertiary butyl hydroquinone.
In this embodiment, the antifreeze agent is propylene glycol.
The preparation method refers to the preparation process of example 1.
Example 8
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
22% of pesticide active agent, 16% of surfactant, 18% of cosolvent, 0.3% of antioxidant, 3% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticidally active agent is sulfoxaflor.
In this embodiment, the surfactant is castor oil ethylene oxide.
In this embodiment, the co-solvent is ethylene glycol diacetate.
In this embodiment, the antioxidant is butylated hydroxyanisole.
In this embodiment, the antifreeze agent is propylene glycol.
The preparation method refers to the preparation process of example 1.
Example 9
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
10% of pesticide active agent, 15% of surfactant, 17% of cosolvent, 0.2% of antioxidant, 3% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agent is nitenpyram.
In this embodiment, the surfactant is phenethylphenol polyoxyethylene ether.
In this embodiment, the co-solvent is ethylene glycol diacetate.
In this embodiment, the antioxidant is butylated hydroxyanisole.
In this embodiment, the antifreeze agent is glycerol.
The preparation method refers to the preparation process of example 1.
Example 10
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
6% of pesticide active agent, 10% of surfactant, 6% of cosolvent, 0.6% of antioxidant, 2% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agent is spinetoram.
In this embodiment, the surfactant is a castor oil ethylene oxide derivative.
In this embodiment, the co-solvent is methyl oleate.
In this embodiment, the antioxidant is butylated hydroxyanisole.
In this embodiment, the antifreeze agent is propylene glycol.
The preparation method refers to the preparation process of example 1.
Example 11
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
24% of pesticide active agent, 13% of surfactant, 11% of cosolvent, 0.4% of antioxidant, 1% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agent is methoxyfenozide.
In this embodiment, the surfactant is a chimeric of an alkyl naphthalene polyoxyethylene and a polyoxypropylene ether.
In this embodiment, the co-solvent is methyl oleate.
In this embodiment, the antioxidant is dibutylhydroxytoluene.
In this embodiment, the antifreeze agent is propylene glycol.
The preparation method refers to the preparation process of example 1.
Example 12
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
10% of pesticide active agent, 11% of surfactant, 14% of cosolvent, 0.05% of antioxidant, 1% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agent is tetrachlorantraniliprole.
In the present embodiment, the surfactant is an alkylnaphthalene polyoxyethylene formaldehyde condensate.
In this embodiment, the co-solvent is methyl oleate.
In this embodiment, the antioxidant is butylated hydroxyanisole.
In this embodiment, the antifreeze agent is glycerol.
The preparation method refers to the preparation process of example 1.
Example 13
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
12% of pesticide active agent, 17% of surfactant, 15% of cosolvent, 0.18% of antioxidant and the balance of neem oil.
In this embodiment, the pesticide active agents are flubendiamide and emamectin benzoate, the flubendiamide is 8%, and the emamectin benzoate is 4%.
In this embodiment, the surfactant is silicone polyoxyethylene ether and castor oil ethylene oxide, and the mass ratio of the silicone polyoxyethylene ether to the castor oil ethylene oxide is 1: 1.
in this embodiment, the co-solvent is ethylene glycol.
In this embodiment, the antioxidant is propyl gallate.
The preparation method refers to the preparation process of example 1.
Example 14
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
30% of pesticide active agent, 20% of surfactant, 12% of cosolvent, 0.18% of antioxidant, 1.5% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agents are imidacloprid and chlorpyrifos, with 5% imidacloprid and 25% chlorpyrifos.
In this embodiment, the surfactant is silicone polyoxyethylene ether and castor oil ethylene oxide, and the mass ratio of the silicone polyoxyethylene ether to the castor oil ethylene oxide is 2: 1.
in this embodiment, the co-solvent is ethylene glycol diacetate.
In this embodiment, the antioxidant is tertiary butyl hydroquinone.
In this embodiment, the antifreeze agent is urea.
The preparation method refers to the preparation process of example 1.
Example 15
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
0.2% of pesticide active agent, 10% of surfactant, 5% of cosolvent, 0.5% of antioxidant and the balance of neem oil.
In this embodiment, the pesticide active agent is emamectin benzoate.
In this embodiment, the surfactant is silicone polyoxyethylene ether.
In this embodiment, the co-solvent is ethylene glycol.
In this embodiment, the antioxidant is butylated hydroxyanisole.
The preparation method refers to the preparation process of example 1.
Example 16
A pesticide special for flying prevention and containing neem oil comprises the following components in percentage by weight:
40% of pesticide active agent, 20% of surfactant, 20% of cosolvent, 0.05% of antioxidant, 1% of antifreeze agent and the balance of neem oil.
In this embodiment, the pesticide active agents are emamectin benzoate and chlorpyrifos, the emamectin benzoate is 1% and the chlorpyrifos is 39%.
In the embodiment, the surfactant is a mixture of castor oil propylene oxide, alkylphenol polyoxyethylene polyoxypropylene ether and fatty alcohol polyoxyethylene ether, and the three are mixed according to the ratio of 1: 1:1, and mixing.
In this embodiment, the cosolvent is isopropanol and methyl oleate, and the mass ratio of isopropanol to methyl oleate is 1: 1.
in this embodiment, the antioxidant is butylated hydroxyanisole.
In this embodiment, the antifreeze agent is urea.
The preparation method refers to the preparation process of example 1.
Biological assay one
1. Indoor bioactivity assay of plutella xylostella
Filter paper was placed in a petri dish (Φ ═ 9cm), and water was added to keep moisture. Directly soaking cabbage leaves in the liquid medicine for 30 seconds, taking out the cabbage leaves with a forceps, airing until no liquid is visible on the surfaces of the leaves, and inoculating test larvae with the same size. Gauze is padded under the culture dish cover, and the culture dish is covered to prevent the test insects from escaping. After the treatment, the culture dish is placed in an insect breeding chamber. And treatment with the corresponding organic solvent without the agent was set as a control. Each treatment was repeated 3 times, with 10 replicates. The death of the test insects was investigated 72 hours after the treatment. The death judgment criteria were: the dead insect was recorded by touching the insect body with a small brush pen.
2. Indoor biological activity assay for rice leaf rollers
A population of rice leaf rollers collected from the field. The collection amount of each population is not less than 300 adult insects. And (3) bringing the collected adults back to a laboratory net room, putting the adults into an insect breeding cage, dipping absorbent cotton into 10% of honey water to supplement nutrition, putting 2-3 pots of rice in a tillering stage into the cage for spawning, preserving moisture in shallow water, and replacing fresh rice plants every day. After the larvae are hatched, 2-instar larvae with the same insect age are selected as test insects.
The toxicity measuring method adopts a leaf soaking stomach toxicity method. Collecting fresh tender green rice leaves at tillering stage, soaking in prepared medicinal liquid with series concentration for 10s, placing on a holder, air drying until no residual water drop can be observed, inserting into large test tube (aperture about 3cm, length about 20cm) with wet cotton ball at bottom, connecting each test tube with 15-head 2-year larva with small brush pen, sealing with preservative film, puncturing with dissecting needle to ventilate, standing in test tube rack, and culturing in light constant temperature incubator (26 + -1 deg.C, light irradiation of 14h/d, relative humidity of 70%). Each treatment was repeated 4 times. Larval mortality was observed and recorded after 3d (72h) rearing. Death of the larvae can be judged by gentle stimulation of the larvae with a probe or dissecting needle without significant action.
3. Indoor toxicity assay for rice planthopper
Digging rice plants from mulberry stage to booting stage with roots, cutting into rice stems of about 10cm long, and reserving root systems of a certain length, 3 plants and 1 group. Soaking rice stem in the prepared medicinal liquid for 30s, taking out, air drying, wrapping the root with absorbent cotton soaked with clear water, and placing into a disposable plastic cup. The 3-year-old midterm nymphs with consistent standards are sucked from potted rice and placed in plastic cups placed horizontally and laterally, 20 heads are placed in each cup, the concentration is repeated for 3 times, 60 heads in total, and the control is treated by clear water. And (3) after inoculation, placing the disposable plastic cup into a constant temperature incubator, wherein the temperature is 26 +/-1 ℃, and the photoperiod is L: D: 16h:8 h. The death of the test insects was checked 72h after the treatment.
4. Indoor toxicity determination of cabbage caterpillar
The leaf soaking method is adopted. Collecting cabbage caterpillar eggs and larvae which are hatched initially from the field, feeding the cabbage caterpillar eggs and the larvae with cabbage leaves indoors, and then selecting healthy larvae with proper ages for testing. Soaking cabbage leaves in the prepared liquid medicine for 3s, putting the leaves into culture dishes padded with wet filter paper after the solvent is completely volatilized, and putting 2 leaves into each dish. Then 3 cabbage caterpillars of 3 ages starved for 4h are placed in each dish, each treatment is repeated for 10 times, and acetone is used for blank control instead of medicinal liquid.
And observing the death condition of the test insects 24 hours after the pesticide is applied.
Figure BDA0003278186430000151
Figure BDA0003278186430000152
The LC of each medicament is obtained through the linear regression analysis between the rate value of the control effect and the logarithm value of the series concentration50The activity of the test agent on the test subject was evaluated by calculating the co-toxicity coefficient (CTC) of the combination by the Sun Yunpei method. The co-toxicity coefficient (CTC) of the compound preparation is more than or equal to 120, which shows a synergistic effect; CTC is less than or equal to 80 and shows antagonism; 80 < CTC < 120 showed additive effects.
TABLE 1 indoor toxicity assay for 3 rd larva of diamondback moth by mixing chlorfenapyr and neem oil
Figure BDA0003278186430000153
a represents chlorfenapyr; b represents neem oil
LC for determining 72h toxicity of chlorfenapyr, nim oil and mixture ratio of chlorfenapyr and nim oil (1:1, 1:2, 1:4, 1:8 and 1:16) after treating 3-instar larvae of diamondback moth50Values of 2.43mg/L, 13192.06mg/L, 4.06mg/L, 5.52mg/L, 8.46mg/L, 28.77mg/L and 37.75mg/L, respectively; the co-toxicity coefficients of the chlorfenapyr and the neem oil in the mixture ratio of (1:1, 1:2, 1:4, 1:8 and 1:16) are 119.70, 132.29, 143.77, 76.01 and 109.26 respectively. From the above results, the ratio of chlorfenapyr to neem oil is 1:2, 1:4 and 1:4 have obvious synergistic effect.
TABLE 2 indoor toxicity assay for 3 rd larva of cabbage caterpillar by mixing beta-cypermethrin with neem oil
Figure BDA0003278186430000161
a represents beta-cypermethrin; b represents neem oil
LC for 24h toxicity determination after 3 rd larva of cabbage caterpillar is treated by beta-cypermethrin, neem oil, beta-cypermethrin and neem oil in the ratio of 1:3, 1:6, 1:9, 1:12 and 1:1850Values of 0.83mg/L, 27530.54mg/L, 2.21mg/L, 4.29mg/L, 2.97mg/L, 9.63mg/L and 15.50mg/L, respectively; the co-toxicity coefficients of the beta-cypermethrin and the neem oil in the mixture ratio of (1:3, 1:6, 1:9, 1:12 and 1:18) are 151.23, 136.01, 280.71, 112.57 and 102.19 respectively. From the above results, it can be seen that the effective cypermethrin and neem oil have obvious synergistic effect when the ratio of the cypermethrin to the neem oil is 1:3, 1:6 and 1: 9.
TABLE 3 indoor toxicity assay for 3 rd larvae of diamondback moth using methoxyfenozide and neem oil in combination
Figure BDA0003278186430000162
Figure BDA0003278186430000171
a represents methoxyfenozide; b represents neem oil
LC for measuring toxicity of 48h after the 3 rd larva of the plutella xylostella is treated by methoxyfenozide, neem oil, methoxyfenozide and neem oil in the mixture ratio of (2:1, 2:5, 2:10, 2:15 and 2:20)50Values of 0.75mg/L, 14941.03mg/L, 1.00mg/L, 1.71mg/L, 3.51mg/L, 4.00mg/L and 7.86mg/L, respectively; the co-toxicity coefficients of the methoxyfenozide and the neem oil in the mixture ratio of (2:1, 2:5, 2:10, 2:15 and 2:20) are respectively 112.13, 153.90, 128.13, 159.45 and 104.86. From the above results, it is known that the ratio of methoxyfenozide and neem oil is 2:5, 2:10 and 2:15, which has obvious synergistic effect.
TABLE 4 indoor toxicity assay of lufenuron and neem oil mixed pairing to 3 rd larvae of diamondback moth
Figure BDA0003278186430000172
Figure BDA0003278186430000181
a represents lufenuron; b represents neem oil
LC for measuring toxicity of 48h after the lufenuron, the neem oil, the lufenuron and the neem oil are respectively proportioned (10:20, 10:15, 10:10, 10:5 and 10:1) to 3-year-old larvae of diamondback moth50Values of 0.45mg/L, 18029.19mg/L, 1.08mg/L, 0.87mg/L, 0.52mg/L, 0.60mg/L and 0.46mg/L, respectively; the co-toxicity coefficients of the lufenuron and the neem oil in the mixture ratio of 10:20, 10:15, 10:10, 10:5 and 10:1 are 124.44, 128.33, 171.63, 112.95 and 107.05 respectively. From the above results, it can be seen that the ratio of lufenuron to neem oil is 10:20, 10:15, and 10:10, which have significant synergistic effects.
TABLE 5 indoor toxicity assay for 3 rd instar larvae of diamondback moth by mixing cyantraniliprole and neem oil
Figure BDA0003278186430000182
a represents cyantraniliprole; b represents neem oil
LC for measuring toxicity of 48h after cyanogen cyantraniliprole, neem oil, cyanogen cyantraniliprole and neem oil are respectively proportioned (1:99, 1:80, 1:60, 1:40 and 1:20) to 3-instar larvae of diamondback moth50Values of 0.86mg/L, 13442.27mg/L, 46.35mg/L, 56.70mg/L, 47.78mg/L, 74.79mg/L and 34.78mg/L, respectively; the co-toxicity coefficients of the cyantraniliprole and the neem oil in the mixture ratio of 1:99, 1:80, 1:60, 1:40 and 1:20 are 184.99, 122.62, 109.72, 47.18 and 52.04 respectively. From the above results, it can be seen that the mixture ratio of cyantraniliprole to neem oil is 1:99 and 1:80, which has obvious synergistic effect.
TABLE 6 indoor toxicity assay for 3 rd larvae of diamondback moth in a cocktail of spinetoram and neem oil
Figure BDA0003278186430000191
a represents spinetoram; b represents neem oil
LC for measuring toxicity of spinetoram, neem oil, spinetoram and neem oil in a ratio of (1:5, 2:5, 3:5, 4:5 and 5:5) after treatment of 3-instar larvae of plutella xylostella for 48 hours50Values of 0.81mg/L, 9148.34mg/L, 3.14mg/L, 1.38mg/L, 1.27mg/L, 1.58mg/L and 1.84mg/L, respectively; the co-toxicity coefficients of the spinetoram and the neem oil in the mixture ratio of (1:5, 2:5, 3:5, 4:5 and 5:5) are 155.46, 206.72, 170.40, 116.12 and 88.28 respectively. From the above results, it can be seen that the spinetoram and neem oil have obvious synergistic effects when the ratio of spinetoram to neem oil is 1:5, 2:5 and 3: 5.
TABLE 7 indoor toxicity assay for 3 rd instar larvae of diamondback moth by mixing indoxacarb and neem oil
Figure BDA0003278186430000201
a represents indoxacarb; b represents neem oil
Indancarb, neem oil, and LC (liquid chromatography) for measuring toxicity of 48h after 3-instar larvae of diamondback moth are treated according to the ratio of indoxacarb to neem oil to the mixture of indoxacarb to neem oil (10:1, 10:2, 10:3, 10:4 and 10:5)50Values of 2.50mg/L, 14941.40mg/L, 2.06mg/L, 1.70mg/L, 1.98mg/L, 2.60mg/L and 3.03mg/L, respectively; the co-toxicity coefficients of the indoxacarb and the neem oil in the mixture ratio of 10:1, 10:2, 10:3, 10:4 and 10:5 are 133.39, 176.31, 164.12, 134.40 and 123.58 respectively. From the above results, it is known that the ratio of indoxacarb to neem oil is 10:1, 10:2, 10:3, 10:4 and 10:5, which has obvious synergistic effect.
TABLE 8 indoor toxicity assay for 3 rd larvae of diamondback moth by mixing emamectin benzoate and neem oil
Figure BDA0003278186430000211
a represents emamectin benzoate; b represents neem oil
LC for determining toxicity of 48h after treatment of 3 rd larvae of diamondback moth in each ratio of emamectin benzoate, neem oil, emamectin benzoate and neem oil (1:99, 1:80, 1:60, 1:40 and 1:20)50Values of 0.14mg/L, 11647.17mg/L, 11.13mg/L, 9.08mg/L, 4.69mg/L, 4.04mg/L and 3.79mg/L, respectively; the co-toxicity coefficients of the emamectin benzoate and the neem oil in the mixture ratio of 1:99, 1:80, 1:60, 1:40 and 1:20 are 123.47, 122.57, 178.74, 139.67 and 76.21 respectively. From the above results, it can be seen that the emamectin benzoate and neem oil ratios of 1:99, 1:80, 1:60 and 1:40 have significant synergistic effects.
TABLE 9 indoor toxicity assay for Tetrachloropyrad and Neem oil mixed paired rice leaf roller 2-instar larvae
Figure BDA0003278186430000212
Figure BDA0003278186430000221
a represents tetrachlorantraniliprole; b represents neem oil
LC for measuring toxicity of 48h after tetrachloro-worm amide, neem oil, tetrachloro-worm amide and neem oil are respectively proportioned (9:1, 6:1, 3:1, 5:4 and 2:5) to 2-instar larvae of cnaphalocrocis medinalis guenee50Values of 0.41mg/L, 1708.29mg/L, 0.54mg/L, 0.73mg/L, 0.51mg/L, 0.58mg/L and 0.90mg/L, respectively; the co-toxicity coefficients of the tetrachloro-zoon amide and the neem oil in the mixture ratio of (9:1, 6:1, 3:1, 5:4 and 2:5) are respectively 84.16, 65.59, 106.81, 128.65 and 160.17. From the above results, it can be seen that the ratio of tetrachlorantraniliprole to neem oil is 5:4 and 2:5, which has significant synergistic effect.
TABLE 10 indoor toxicity assay for 3 rd instar midterm nymphs of rice planthoppers by combining thiamethoxam and neem oil
Figure BDA0003278186430000222
a represents thiamethoxam; b represents neem oil
LC for determining 72h toxicity of thiamethoxam, neem oil, thiamethoxam and neem oil in a ratio of 1:5, 1:10, 1:20, 1:40 and 1:80 after treatment of 3-year-old mid-term nymphs of rice planthoppers50Values of 0.22mg/L, 12781.98mg/L, 1.31mg/L, 2.23mg/L, 2.88mg/L, 6.31mg/L and 29.88mg/L, respectively; the co-toxicity coefficients of the thiamethoxam and the neem oil in the mixture ratio of 1:5, 1:10, 1:20, 1:40 and 1:80 are 101.64, 109.23, 161.58, 144.03 and 60.08 respectively. From the above results, the ratio of thiamethoxam to neem oil is 1:20 and 1:40 has obvious synergistic effect.
And (2) biological activity determination: test of field drug effect
1. The investigation time and method of cabbage caterpillar comprises the following steps: the investigation is carried out 1 time respectively before the application of the pesticide and 1 day, 3 days and 7 days after the application of the pesticide, a five-point sampling method is adopted for the investigation, 5 cabbage hearts are fixedly investigated at each point, 25 cabbage hearts are investigated in each cell, the number of live insects is recorded, and the decline rate and the control effect are calculated.
Relative control efficacy was calculated compared to the placebo zone. Calculated according to the following formula:
Figure BDA0003278186430000231
in the formula: CK0 is before drug administration in control area; CK1 is after control area drug administration;
pt0 is before treatment area; pt1 is after treatment area drug;
the using dosage of the example 1 (4.5% of the special pesticide for preventing the oil flying of the cypermethrin-neem) and the control pesticide (4.5% of the aqueous emulsion of the cypermethrin) is 45 mL/mu, the water consumption is 1L/mu, the flying height is 2.0m, and the flying speed is 3m/s, so that the results show that the control effect of the example 1 on cabbage caterpillar is better than that of the control pesticide in 1, 3 and 7 days, and particularly the control pesticide is obviously different from the control pesticide in 1 and 7 days. The results are shown in FIG. 1.
2. The Spodoptera frugiperda investigation time and method comprise the following steps: investigation is carried out 1 time respectively before application and 1 day, 3 days and 7 days after application, 5 points are taken according to a Z shape in each cell, 10 corns are marked on each point, 50 corns are investigated totally, the number of live insects on the corn plants is recorded, and the condition of phytotoxicity is observed.
Relative control efficacy was calculated compared to the placebo zone. Calculated according to the following formula:
Figure BDA0003278186430000241
Figure BDA0003278186430000242
the using dosage of the example 3 (10% of the chlorfenapyr neem oil flying prevention special medicament) and the control medicament (10% of the chlorfenapyr suspending agent) for spodoptera frugiperda is 40 mL/mu, the water consumption is 1L/mu, the flying height is 1.8m, and the flying speed is 3m/s, so that the results show that the control effect of the example 3 on spodoptera frugiperda is better than that of the control medicament in 1, 3 and 7 days, particularly the 1 st day and the 3 rd day. The results are shown in FIG. 2.
3. Time and method for investigating rice planthopper. The population base of the insects was investigated before application, and the number of live insects was investigated 3, 7 and 14 days after application. And (3) surveying 25 points and 2 clusters in each treatment area by a parallel jumping method, wherein in the survey, a white porcelain plate is firstly placed at the base part of the rice, then the rice clusters 2 are beaten towards the direction of the white porcelain plate, so that the rice planthoppers fall into the porcelain plate, the number of the rice planthoppers on the white porcelain plate is counted, and the insect population reduction rate and the prevention effect are calculated.
The calculation formula is as follows:
Figure BDA0003278186430000243
Figure BDA0003278186430000244
in example 14 (30% imidacloprid and chlorpyrifos oil special-purpose pesticide) and a control pesticide (30% imidacloprid and chlorpyrifos microemulsion), the dosage per mu of the rice planthopper is 40 mL/mu, the water consumption is 1L/mu, the flying height is 2.0m, and the flying speed is 3m/s, and the results show that the quick-acting property and the lasting effect of example 14 are better than those of the control pesticide, and the control effect of 3 days after pesticide application and 14 days after pesticide application is obviously different from that of the control pesticide. The results are shown in FIG. 3.
4. The cotton aphid pesticide effect test investigation time and method are as follows: according to the experimental design, sampling is carried out at 2 rows and 5 points in the middle of each cell, 2 plants are fixed at each point, and 3 aphid leaves are investigated on the upper part of each fixed plant. The number of surviving insects was investigated before and 1d, 3d and 10d after the drug. A data processing method.
Figure BDA0003278186430000251
Figure BDA0003278186430000252
In example 8 (22% flonicamid neem oil special-purpose pesticide) and a control pesticide (22% flonicamid suspension) with the dosage of 15 mL/mu, the water consumption of 1L/mu, the flying height of 1.8m and the flying speed of 3m/s for cotton aphids, the result shows that the persistent effect of example 8 is better than that of the control pesticide, the control effect of the control pesticide is equivalent to that of the control pesticide 1 day after the pesticide application, and the control effect of the cotton aphids 10 days after the pesticide application is significantly different from that of the control pesticide. The results are shown in FIG. 4.
Evaluation of anti-Drift ability of the agents of examples
The flying prevention agent prepared in examples 1 to 15 and water were mixed with a mixture of 1: 100 are mixed to prepare spraying liquid for pesticide application, the water consumption per mu is 1L/mu, the flying height is 2m away from the ground, the flying speed is 3m/s, pesticide application is carried out under the condition that the wind speed is 0.9 m/s-2.8 m/s, the flying direction is vertical to the wind direction, 30 plastic culture dishes with the diameter of 15cm are placed in 3 groups of 10 culture dishes per 10m according to 3, 4 and 3 in the lower wind port direction of the flight line of an airplane and the vertical distance from the flight line is 0-10m, 10-20m and 20-30m, and drift is collected. As can be seen from the results in the table, the environment-friendly emulsifiable concentrate prepared by using the neem oil for the unmanned aerial vehicle has better anti-drift capability, the drift rate of 0-10m on the ground is 3.2-26.5%, the drift rate of 10-20m is 0.8-17.5%, the drift rate of 20-30m is 0.0-10.6%, and the drift rate of 20-30m is below 10% except for example 8. The results, which show the relatively good anti-drift efficiency of the examples, are shown in Table 11.
TABLE 11 anti-drifting ability of the liquid medicine of examples
Figure BDA0003278186430000261
The above description is only for the preferred embodiment of the present invention, but the present invention should not be limited to the embodiment and the disclosure of the drawings, and therefore, all equivalent or modifications that do not depart from the spirit of the present invention are intended to fall within the scope of the present invention.

Claims (7)

1. A special pesticide containing neem oil for flying prevention is characterized by comprising the following components in percentage by weight: 0.2-40% of pesticide active agent, 10-25% of surfactant, 5-20% of cosolvent, 0.05-1% of antioxidant and the balance of neem oil.
2. The neem oil-containing agricultural chemical for flying prevention according to claim 1, wherein: the anti-freezing agent also comprises 0.001-5% by weight, and the anti-freezing agent comprises one or more than two of glycerol, propylene glycol and urea.
3. The neem oil-containing agricultural chemical for flying prevention according to claim 1, wherein: the pesticide active agent comprises one or more of chlorantraniliprole, emamectin benzoate, cyantraniliprole, tetrachlorantraniliprole, beta-cypermethrin, lufenuron, methoxyfenozide, indoxacarb, imidacloprid, chlorfenapyr, flubendiamide, spinetoram, nitenpyram, chlorpyrifos, hexaflumuron, sulfoxaflor and acetamiprid.
4. The neem oil-containing agricultural chemical for flying prevention according to claim 1, wherein: the surfactant comprises one or more of organic silicon polyoxyethylene ether, fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, castor oil ethylene oxide derivatives, castor oil propylene oxide derivatives, alkylphenol polyoxyethylene polyoxypropylene ether, chimera of alkylphenol polyoxyethylene and polyoxypropylene ether, alkylphenol polyoxyethylene formaldehyde condensate, alkyl biphenol polyoxyethylene polyoxypropylene ether, chimera of alkyl biphenol polyoxyethylene and polyoxypropylene ether, alkyl biphenol polyoxyethylene formaldehyde condensate, alkyl naphthalene polyoxyethylene polyoxypropylene ether, chimera of alkyl naphthalene polyoxyethylene and polyoxypropylene ether or alkyl naphthalene polyoxyethylene formaldehyde condensate.
5. The neem oil-containing agricultural chemical for flying prevention according to claim 1, wherein: the cosolvent comprises one or more of ethylene glycol diacetate, ethylene glycol, isopropanol and methyl oleate.
6. The neem oil-containing agricultural chemical for flying prevention according to claim 1, wherein: the antioxidant comprises one or more of propyl gallate, butyl hydroxy anisol, dibutyl hydroxy toluene, and tert-butyl hydroquinone.
7. A preparation method of the pesticide containing neem oil specially used for flying defense as claimed in any one of claims 1 to 6, characterized in that the preparation method comprises the following steps:
s1, adding heat conducting oil into the reaction kettle and heating to dry the interior of the reaction kettle;
s2, adding a cosolvent into a dry and anhydrous reaction kettle, then adding a pesticide active agent, and stirring at the rotating speed of 1000-1500r/min for 10-20 min;
s3, adding a surfactant into the reaction kettle, and continuously stirring for 10-15 min;
s4, adding neem oil into the reaction kettle, and continuously stirring for 10-15 min;
s5, adding an antioxidant into the reaction kettle, and continuously stirring for 5-10 min;
s6, adding an antifreeze agent into the reaction kettle, and continuously stirring for 5-10 min;
and S7, naturally cooling to room temperature after stirring.
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