CN113748902A - Method for removing overwintering aphids of goldenrain tree - Google Patents
Method for removing overwintering aphids of goldenrain tree Download PDFInfo
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- CN113748902A CN113748902A CN202111176080.2A CN202111176080A CN113748902A CN 113748902 A CN113748902 A CN 113748902A CN 202111176080 A CN202111176080 A CN 202111176080A CN 113748902 A CN113748902 A CN 113748902A
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- 241001124076 Aphididae Species 0.000 title claims abstract description 56
- 241000167847 Koelreuteria paniculata Species 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 21
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- 230000002265 prevention Effects 0.000 claims abstract description 32
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
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- 238000002156 mixing Methods 0.000 claims description 14
- 238000000967 suction filtration Methods 0.000 claims description 14
- 229920000858 Cyclodextrin Polymers 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000001116 FEMA 4028 Substances 0.000 claims description 11
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 11
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 11
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 11
- 229960004853 betadex Drugs 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 10
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- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 235000009518 sodium iodide Nutrition 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- JSNRRGGBADWTMC-UHFFFAOYSA-N (6E)-7,11-dimethyl-3-methylene-1,6,10-dodecatriene Chemical compound CC(C)=CCCC(C)=CCCC(=C)C=C JSNRRGGBADWTMC-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
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- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 18
- 241000196324 Embryophyta Species 0.000 description 17
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 14
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 description 14
- 239000002253 acid Substances 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
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- DGJMPUGMZIKDRO-UHFFFAOYSA-N cyanoacetamide Chemical compound NC(=O)CC#N DGJMPUGMZIKDRO-UHFFFAOYSA-N 0.000 description 7
- 239000003814 drug Substances 0.000 description 7
- OCJKUQIPRNZDTK-UHFFFAOYSA-N ethyl 4,4,4-trifluoro-3-oxobutanoate Chemical compound CCOC(=O)CC(=O)C(F)(F)F OCJKUQIPRNZDTK-UHFFFAOYSA-N 0.000 description 7
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 description 6
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- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
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- 238000002390 rotary evaporation Methods 0.000 description 3
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- 238000006467 substitution reaction Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 241000131068 Coccinella septempunctata Species 0.000 description 2
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- 238000004132 cross linking Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical group O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 2
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- 235000006029 Prunus persica var nucipersica Nutrition 0.000 description 1
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- 235000013601 eggs Nutrition 0.000 description 1
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
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- 238000007344 nucleophilic reaction Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G13/00—Protecting plants
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
- A01G7/00—Botany in general
- A01G7/06—Treatment of growing trees or plants, e.g. for preventing decay of wood, for tingeing flowers or wood, for prolonging the life of plants
-
- 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
- A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
-
- 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
- A01N27/00—Biocides, pest repellants or attractants, or plant growth regulators containing hydrocarbons
-
- 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
- A01N29/00—Biocides, pest repellants or attractants, or plant growth regulators containing halogenated hydrocarbons
- A01N29/02—Acyclic compounds or compounds containing halogen attached to an aliphatic side-chain of a cycloaliphatic ring system
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Environmental Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Dentistry (AREA)
- Pest Control & Pesticides (AREA)
- Zoology (AREA)
- Agronomy & Crop Science (AREA)
- Toxicology (AREA)
- Plant Pathology (AREA)
- Biodiversity & Conservation Biology (AREA)
- Ecology (AREA)
- Forests & Forestry (AREA)
- Botany (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a method for removing overwintering aphids of goldenrain trees in Mount Huang, which comprises the following steps: step one, ecological prevention and control; secondly, physical prevention and control; thirdly, biological prevention and control; suspending the ladybug phagostimulant at a position 3-5cm higher than an action target in the aphid group in the month of 4, wherein the distance between every two ladybug phagostimulants is 10cm, and releasing the seed ladybugs in the aphid group; fourthly, chemical prevention and control; the prevention and control of overwintering aphids are carried out comprehensively by four prevention and control means of ecology, physics, biology and chemistry, the ecological prevention and control is firstly carried out, the biological compound fertilizer is applied, the special compound formula of the prevention and control method provides nutrition required by planting of the goldenrain denrain trees on one hand, and a biological prevention and control and soil-borne disease mechanism can be formed on the other hand.
Description
Technical Field
The invention belongs to the technical field of plant pest control, and particularly relates to a method for controlling overwintering aphids of goldenrain trees.
Background
Aphids, also known as greates and nectarines, are a group of phytophagous insects, including all members of the aphid superfamily (also known as aphid superfamily). A total of 10 aphids have been found, of which there are about 4400, most of which belong to the Aphididae family. Aphids are among the most destructive pests. About 250 of them are harmful pests to agriculture, forestry and gardening. The aphid breeding and adaptability are strong, the effect of radical cure is difficult to achieve by a conventional chemical prevention and control method, and the chemical pesticide is used in a large amount, so that agricultural pests generally have drug resistance, and the aphids are in a hibernation and overwintering state in the late winter, so that the prevention and control means of overwintering aphids are made in the autumn and winter of the previous year, and the outbreak of the aphids in the spring of the next year can be effectively reduced.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method for controlling overwintering aphids of goldenrain trees.
The purpose of the invention can be realized by the following technical scheme:
a method for controlling overwintering aphids of goldenrain trees comprises the following steps:
step one, ecological prevention and control;
applying biological compound fertilizer to the goldenrain tree in 9 months, controlling the application once every half month, and applying 10-12kg per mu;
secondly, physical prevention and control;
the method comprises the following steps of scraping old and beautiful barks of the trunk of the goldenrain tree in 10-11 months and whitewashing the trunk and backbone boughs of the goldenrain tree by using a whitewash agent;
thirdly, biological prevention and control;
suspending the ladybug phagostimulant at a position 3-5cm higher than an action target in the aphid group in the month of 4, wherein the distance between every two ladybug phagostimulants is 10cm, and releasing the seed ladybugs in the aphid group;
and fourthly, chemical prevention and treatment.
Furthermore, the biological compound fertilizer is prepared by mixing the defluorinate, the HYT-A strain agent and the HYT-B strain agent according to the weight ratio of 1: 0.2-0.5: 0.3-0.5.
Further, the ladybug phagostimulant is prepared by the following steps:
step S1, adding beta-cyclodextrin into deionized water, slowly dropwise adding a sodium hydroxide aqueous solution with the concentration of 8mol/L, and uniformly stirring after dropwise adding is finished until a system is clear to prepare a solution a; adding paratoluensulfonyl chloride into acetonitrile, and stirring at a constant speed until the mixture is dissolved to prepare a solution b; dropwise adding the solution b into the solution a, uniformly stirring at room temperature, reacting for 2h, performing suction filtration, removing filter residues, dropwise adding dilute hydrochloric acid with the mass fraction of 10% to adjust the pH until the pH is 6, and performing cold preservation at 5 ℃ for 12h to obtain an intermediate 1, wherein the dosage ratio of beta-cyclodextrin, sodium hydroxide aqueous solution and deionized water is controlled to be 60 g: 20 mL: 500mL, the dosage ratio of p-toluenesulfonyl chloride and acetonitrile is 10.05 g: 35mL, and the volume ratio of the solution b to the solution a is 1: 12-15;
step S1, respectively preparing beta-cyclodextrin and p-toluenesulfonyl chloride into solutions, then mixing and reacting, carrying out nucleophilic reaction on p-toluenesulfonyl chloride and beta-cyclodextrin, and replacing hydroxyl on the beta-cyclodextrin with p-toluenesulfonyl chloride to prepare an intermediate 1;
step S2, adding the intermediate 1, sodium iodide and ethylenediamine into a flask, dropwise adding N-methyl pyrrolidone, introducing nitrogen after completely adding, heating to 95 ℃, stirring at a constant speed and reacting for 5 hours, transferring into absolute ethyl alcohol after the reaction is finished, standing until a precipitate is separated out, performing suction filtration to obtain a primary material, then adding deionized water, stirring at a constant speed and adding pheromone, continuing stirring for 15 minutes, then adding hydroxyethyl cellulose, performing ultrasonic treatment for 30 minutes to obtain a ladybug attractant, wherein the dosage ratio of the intermediate 1, the sodium iodide, the ethylenediamine and the N-methyl pyrrolidone is controlled to be 2.5 g: 0.015 g: 0.35 g: 5mL, and the dosage ratio of the primary material, the pheromone, the deionized water and the hydroxyethyl cellulose is controlled to be 0.25 g: 0.025 g: 5 mL: 0.4 g;
step S2, preparing a primary material, wherein the intermediate 1 and ethylenediamine are subjected to substitution reaction in the preparation process to generate the primary material which is a composition of cyclodextrin and ethylenediamine, then adding pheromone as a coated material, and finally adding hydroxyethyl cellulose to generate the ladybug phagostimulant with the three-dimensional network structure through physical crosslinking; suspending the ladybug phagostimulant in the aphid group, watering the aphid group, and leading the ladybug phagostimulant to absorb water and expand, slowly releasing the internal pheromone, luring the ladybug to gather and killing aphids.
Further: the chemical control comprises the following steps: spraying the preventing and controlling agent to the goldenrain tree in 4-5 months of the year, wherein the time for spraying the preventing and controlling agent is ten o 'clock before the morning or five o' clock after the afternoon.
Further: the prevention and treatment medicament is prepared by the following steps:
step S11, adding ethyl trifluoroacetoacetate and cyanoacetamide into a three-neck flask, adding methanol, heating to 65 ℃ until a clear solution is formed, dropwise adding a potassium hydroxide methanol solution, reacting for 2 hours after dropwise adding, separating out a precipitate, filtering and washing to obtain an intermediate a, and controlling the dosage ratio of the ethyl trifluoroacetoacetate, the cyanoacetamide, the methanol and the potassium hydroxide methanol solution to be 70 g: 32.5 g: 120 mL: 22.5 g;
the potassium hydroxide methanol solution is formed by mixing potassium hydroxide and methanol according to the dosage ratio of 0.35-0.42 mol: 50 mL.
In step S11, ethyl trifluoroacetoacetate and cyanoacetamide react to form intermediate a, the reaction process is as follows:
step S12, adding the intermediate a and tetramethylammonium chloride into triethylamine, stirring at a constant speed, slowly adding phosphorus oxychloride, stirring at a constant speed, heating to reflux, reacting for 8 hours, transferring the generated reaction liquid into ice water, separating out a precipitate to obtain an intermediate b, and controlling the dosage ratio of the intermediate a, the tetramethylammonium chloride, the triethylamine and the phosphorus oxychloride to be 40 g: 21.5-22.0 g: 40 g: 120 mL;
in the step S12, the intermediate a reacts with phosphorus oxychloride to generate an intermediate b, and the reaction process is as follows:
step S13, slowly adding the intermediate b into the mixed acid, maintaining the temperature of the system at 65 ℃, heating to 100 ℃ after completely adding the intermediate b, preserving the temperature, reacting for 2 hours, cooling, pouring the mixture into ice water to precipitate, performing suction filtration and drying to obtain an intermediate c, and controlling the dosage ratio of the intermediate b to the mixed acid to be 20-25 g: 75 mL;
the mixed acid is formed by mixing concentrated sulfuric acid and concentrated nitric acid according to the volume ratio of 5: 1.
Step S14, adding the intermediate c into a three-neck flask, sequentially adding sodium acetate and absolute ethyl alcohol, stirring at a constant speed, adding a catalyst, introducing nitrogen to replace air, introducing hydrogen, stirring at a constant speed, reacting for 8 hours, performing suction filtration, recovering the catalyst, performing rotary evaporation on filtrate to remove the solvent, dissolving the generated solid in deionized water, adjusting the pH to 3, extracting with ethyl acetate, and drying to obtain an intermediate d, wherein the dosage ratio of the intermediate c, the sodium acetate, the absolute ethyl alcohol and the catalyst is controlled to be 5 g: 5.25 g: 30 mL: 0.2 g;
in the step S13, the intermediate b generates an intermediate c under the action of the mixed acid, and then the intermediate c generates an intermediate d under the action of the catalyst and hydrogen, and the reaction process is as follows:
and step S15, adding the intermediate d and thionyl chloride into DMF, stirring at a constant speed for 2 hours, and then adding aminoacetonitrile hydrochloride to prepare the control medicament, wherein the molar ratio of the intermediate d to the thionyl chloride is controlled to be 1: 1.
In the step S15, the intermediate d reacts with thionyl chloride in DMF to generate a control agent, and the reaction process is as follows:
the invention has the beneficial effects that:
the invention comprehensively prevents and treats the overwintering aphids by four prevention and treatment means of ecology, physics, biology and chemistry, firstly prevents and treats the overwintering aphids by the ecology and applies a biological compound fertilizer, the special compound formula of the method provides nutrition required by planting the goldenrain tree, can form a biological control and soil-borne disease mechanism, whitewashes the tree body of the goldenrain tree in 10-11 months, can kill overwintering aphids, but also can prevent aphid from laying eggs and breeding, then the ladybug phagostimulant is hung in the residual aphid group 3-5cm higher than the action target in the next 4 months, in the preparation process of the ladybug phagostimulant, the intermediate 1 and the ethylenediamine are subjected to substitution reaction to generate a primary material, the ladybug phagostimulant is a composition of cyclodextrin and ethylenediamine, pheromone is added as a coated material, and finally hydroxyethyl cellulose is added to generate the ladybug phagostimulant with a three-dimensional network structure through physical crosslinking; suspending the ladybug phagostimulant in the aphid group, watering the aphid group, enabling the ladybug phagostimulant to absorb water and swell, slowly releasing internal pheromone, luring the ladybug to gather, killing aphids, and finally spraying a control agent to carry out chemical control.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Indoor experiments:
taking 4 indoor planted peace tree plants, respectively recording as A, B, C and D, placing in a laboratory, taking D as a control group, respectively connecting 100 indoor raised aphids to plant leaves of A, B, C and D, then placing 10 coccinella septempunctata in the laboratory, hanging the coccinella septempunctata phagostimulant at a position 3-5cm higher than an action target in a A, B, C plant aphid group, investigating the result after taking food for 24 hours, repeating the test for three times, detecting the residual aphid quantity on A, B, C and D plants, and obtaining the result that 30 +/-3.5 plants remain on A, 31 +/-4.2 plants remain on B, 30 +/-4.5 plants remain on C and 96 +/-3.2 plants remain on D.
From example 1, it can be seen that the ladybug phagostimulant of the present invention has a good attractant effect for ladybugs.
Example 2
Indoor experiments:
taking 3 indoor planted peace tree plants, respectively recording as A, B, C, placing in a laboratory, respectively connecting 100 indoor raised aphids to plant leaves A, B, C and D, ten points in the morning, preparing a control medicament into a solvent with the mass fraction of 0.3mmol/L, spraying the solvent on A, B, C plants, investigating the result after eating for 24 hours, repeating the experiment for three times, detecting the residual aphids on A, B, C and D plants, and obtaining the results that 33 +/-4.5 plants are remained on A, 34 +/-4.1 plants are remained on B, 35 +/-3.5 plants are remained on C and 97 +/-2.8 plants are remained on D.
From example 2, it can be seen that the control agents of the present invention have good control effects on aphids.
Outdoor experiments:
selecting a growing area of the goldenrain tree in the same area, dividing the growing area into three areas of example 3, example 4 and comparative example 1, and respectively controlling overwintering aphids of the goldenrain tree in different areas according to the following modes:
example 3
Step one, ecological prevention and control;
applying a biological compound fertilizer to the goldenrain trees in 9 months, controlling the application once every half month, and applying 10kg per mu;
the biological compound fertilizer is prepared by mixing the defluximab, the HYT-A strain agent and the HYT-B strain agent according to the weight ratio of 1: 0.2: 0.3.
Secondly, physical prevention and control;
the method comprises the following steps of scraping old and beautiful barks of the trunk of the goldenrain tree in 10-11 months and whitewashing the trunk and backbone boughs of the goldenrain tree by using a whitewash agent;
thirdly, biological prevention and control;
suspending the ladybug phagostimulant at a position 3cm higher than an action target in the aphid group in the month of 4, wherein the distance between every two ladybug phagostimulants is 10cm, and releasing the seed ladybugs in the aphid group;
the ladybug phagostimulant is prepared by the following steps:
step S1, adding beta-cyclodextrin into deionized water, slowly dropwise adding a sodium hydroxide aqueous solution with the concentration of 8mol/L, and uniformly stirring after dropwise adding is finished until a system is clear to prepare a solution a; adding paratoluensulfonyl chloride into acetonitrile, and stirring at a constant speed until the mixture is dissolved to prepare a solution b; dropwise adding the solution b into the solution a, uniformly stirring at room temperature, reacting for 2h, performing suction filtration, removing filter residues, dropwise adding dilute hydrochloric acid with the mass fraction of 10% to adjust the pH until the pH is 6, and performing cold preservation at 5 ℃ for 12h to obtain an intermediate 1, wherein the dosage ratio of beta-cyclodextrin, sodium hydroxide aqueous solution and deionized water is controlled to be 60 g: 20 mL: 500mL, the dosage ratio of p-toluenesulfonyl chloride and acetonitrile is 10.05 g: 35mL, and the volume ratio of the solution b to the solution a is 1: 12;
step S2, adding the intermediate 1, sodium iodide and ethylenediamine into a flask, dropwise adding N-methyl pyrrolidone, completely adding the N-methyl pyrrolidone, introducing nitrogen, heating to 95 ℃, uniformly stirring and reacting for 5 hours, transferring the mixture into absolute ethyl alcohol after the reaction is finished, standing until a precipitate is separated out, performing suction filtration to obtain a primary material, adding deionized water, uniformly stirring and adding pheromone, continuously stirring for 15 minutes, adding hydroxyethyl cellulose, performing ultrasonic treatment for 30 minutes to obtain the ladybug attractant, wherein the dosage ratio of the intermediate 1, the sodium iodide, the ethylenediamine and the N-methyl pyrrolidone is controlled to be 2.5 g: 0.015 g: 0.35 g: 5mL, and the dosage ratio of the primary material, the pheromone, the deionized water and the hydroxyethyl cellulose is controlled to be 0.25 g: 0.025 g: 5 mL: 0.4 g.
The pheromone is formed by mixing trans-beta-farnesene and cis-3-hexenol according to the weight ratio of 2: 1.
And fourthly, chemical prevention and treatment.
Spraying the preventing and controlling agent to the goldenrain tree in 4-5 months of the year, wherein the time for spraying the preventing and controlling agent is ten o 'clock before the morning or five o' clock after the afternoon.
The prevention and treatment medicament is prepared by the following steps:
step S11, adding ethyl trifluoroacetoacetate and cyanoacetamide into a three-neck flask, adding methanol, heating to 65 ℃ until a clear solution is formed, dropwise adding a potassium hydroxide methanol solution, reacting for 2 hours after dropwise adding, separating out a precipitate, filtering and washing to obtain an intermediate a, and controlling the dosage ratio of the ethyl trifluoroacetoacetate, the cyanoacetamide, the methanol and the potassium hydroxide methanol solution to be 70 g: 32.5 g: 120 mL: 22.5 g;
the potassium hydroxide methanol solution is formed by mixing potassium hydroxide and methanol according to the dosage ratio of 0.35 mol: 50 mL.
Step S12, adding the intermediate a and tetramethylammonium chloride into triethylamine, stirring at a constant speed, slowly adding phosphorus oxychloride, stirring at a constant speed, heating to reflux, reacting for 8 hours, transferring the generated reaction liquid into ice water, separating out a precipitate to obtain an intermediate b, and controlling the dosage ratio of the intermediate a, the tetramethylammonium chloride, the triethylamine and the phosphorus oxychloride to be 40 g: 21.5 g: 40 g: 120 mL;
step S13, slowly adding the intermediate b into the mixed acid, maintaining the temperature of the system at 65 ℃, heating to 100 ℃ after completely adding the intermediate b, preserving the temperature, reacting for 2 hours, cooling, pouring the mixture into ice water to precipitate, performing suction filtration and drying to obtain an intermediate c, and controlling the dosage ratio of the intermediate b to the mixed acid to be 20 g: 75 mL;
the mixed acid is formed by mixing concentrated sulfuric acid and concentrated nitric acid according to the volume ratio of 5: 1.
Step S14, adding the intermediate c into a three-neck flask, sequentially adding sodium acetate and absolute ethyl alcohol, stirring at a constant speed, adding a palladium-carbon catalyst, introducing nitrogen to replace air, introducing hydrogen, stirring at a constant speed, reacting for 8 hours, performing suction filtration, recovering the catalyst, performing rotary evaporation on filtrate to remove the solvent, dissolving the generated solid in deionized water, adjusting the pH to 3, extracting with ethyl acetate, and drying to obtain an intermediate d, wherein the dosage ratio of the intermediate c, the sodium acetate, the absolute ethyl alcohol and the palladium-carbon catalyst is controlled to be 5 g: 5.25 g: 30 mL: 0.2 g;
and step S15, adding the intermediate d and thionyl chloride into DMF, stirring at a constant speed for 2 hours, and then adding aminoacetonitrile hydrochloride to prepare the control medicament, wherein the molar ratio of the intermediate d to the thionyl chloride is controlled to be 1: 1.
Example 4
Step one, ecological prevention and control;
applying a biological compound fertilizer to the goldenrain trees in 9 months, controlling the application once every half month, and applying 12kg per mu;
the biological compound fertilizer is prepared by mixing the defluximab, the HYT-A strain agent and the HYT-B strain agent according to the weight ratio of 1: 0.5.
Secondly, physical prevention and control;
the method comprises the following steps of scraping old and beautiful barks of the trunk of the goldenrain tree in 10-11 months and whitewashing the trunk and backbone boughs of the goldenrain tree by using a whitewash agent;
thirdly, biological prevention and control;
suspending the ladybug phagostimulant at a position 5cm higher than an action target in the aphid group in the month of 4, wherein the distance between every two ladybug phagostimulants is 10cm, and releasing the seed ladybugs in the aphid group;
the ladybug phagostimulant is prepared by the following steps:
step S1, adding beta-cyclodextrin into deionized water, slowly dropwise adding a sodium hydroxide aqueous solution with the concentration of 8mol/L, and uniformly stirring after dropwise adding is finished until a system is clear to prepare a solution a; adding paratoluensulfonyl chloride into acetonitrile, and stirring at a constant speed until the mixture is dissolved to prepare a solution b; dropwise adding the solution b into the solution a, uniformly stirring at room temperature, reacting for 2h, performing suction filtration, removing filter residues, dropwise adding dilute hydrochloric acid with the mass fraction of 10% to adjust the pH until the pH is 6, and performing cold preservation at 5 ℃ for 12h to obtain an intermediate 1, wherein the dosage ratio of beta-cyclodextrin, sodium hydroxide aqueous solution and deionized water is controlled to be 60 g: 20 mL: 500mL, the dosage ratio of p-toluenesulfonyl chloride and acetonitrile is 10.05 g: 35mL, and the volume ratio of the solution b to the solution a is 1: 15;
step S2, adding the intermediate 1, sodium iodide and ethylenediamine into a flask, dropwise adding N-methyl pyrrolidone, completely adding the N-methyl pyrrolidone, introducing nitrogen, heating to 95 ℃, uniformly stirring and reacting for 5 hours, transferring the mixture into absolute ethyl alcohol after the reaction is finished, standing until a precipitate is separated out, performing suction filtration to obtain a primary material, adding deionized water, uniformly stirring and adding pheromone, continuously stirring for 15 minutes, adding hydroxyethyl cellulose, performing ultrasonic treatment for 30 minutes to obtain the ladybug attractant, wherein the dosage ratio of the intermediate 1, the sodium iodide, the ethylenediamine and the N-methyl pyrrolidone is controlled to be 2.5 g: 0.015 g: 0.35 g: 5mL, and the dosage ratio of the primary material, the pheromone, the deionized water and the hydroxyethyl cellulose is controlled to be 0.25 g: 0.025 g: 5 mL: 0.4 g.
The pheromone is formed by mixing trans-beta-farnesene and cis-3-hexenol according to the weight ratio of 2: 1.
And fourthly, chemical prevention and treatment.
Spraying the preventing and controlling agent to the goldenrain tree in 4-5 months of the year, wherein the time for spraying the preventing and controlling agent is ten o 'clock before the morning or five o' clock after the afternoon.
The prevention and treatment medicament is prepared by the following steps:
step S11, adding ethyl trifluoroacetoacetate and cyanoacetamide into a three-neck flask, adding methanol, heating to 65 ℃ until a clear solution is formed, dropwise adding a potassium hydroxide methanol solution, reacting for 2 hours after dropwise adding, separating out a precipitate, filtering and washing to obtain an intermediate a, and controlling the dosage ratio of the ethyl trifluoroacetoacetate, the cyanoacetamide, the methanol and the potassium hydroxide methanol solution to be 70 g: 32.5 g: 120 mL: 22.5 g;
the potassium hydroxide methanol solution is formed by mixing potassium hydroxide and methanol according to the dosage ratio of 0.42 mol: 50 mL.
Step S12, adding the intermediate a and tetramethylammonium chloride into triethylamine, stirring at a constant speed, slowly adding phosphorus oxychloride, stirring at a constant speed, heating to reflux, reacting for 8 hours, transferring the generated reaction liquid into ice water, separating out a precipitate to obtain an intermediate b, and controlling the dosage ratio of the intermediate a, the tetramethylammonium chloride, the triethylamine and the phosphorus oxychloride to be 40 g: 22.0 g: 40 g: 120 mL;
step S13, slowly adding the intermediate b into the mixed acid, maintaining the temperature of the system at 65 ℃, heating to 100 ℃ after completely adding the intermediate b, preserving the temperature, reacting for 2 hours, cooling, pouring the mixture into ice water to precipitate, performing suction filtration and drying to obtain an intermediate c, and controlling the dosage ratio of the intermediate b to the mixed acid to be 25 g: 75 mL;
the mixed acid is formed by mixing concentrated sulfuric acid and concentrated nitric acid according to the volume ratio of 5: 1.
Step S14, adding the intermediate c into a three-neck flask, sequentially adding sodium acetate and absolute ethyl alcohol, stirring at a constant speed, adding a palladium-carbon catalyst, introducing nitrogen to replace air, introducing hydrogen, stirring at a constant speed, reacting for 8 hours, performing suction filtration, recovering the catalyst, performing rotary evaporation on filtrate to remove the solvent, dissolving the generated solid in deionized water, adjusting the pH to 3, extracting with ethyl acetate, and drying to obtain an intermediate d, wherein the dosage ratio of the intermediate c, the sodium acetate, the absolute ethyl alcohol and the palladium-carbon catalyst is controlled to be 5 g: 5.25 g: 30 mL: 0.2 g;
and step S15, adding the intermediate d and thionyl chloride into DMF, stirring at a constant speed for 2 hours, and then adding aminoacetonitrile hydrochloride to prepare the control medicament, wherein the molar ratio of the intermediate d to the thionyl chloride is controlled to be 1: 1.
Comparative example 1
Compared with example 3, the overwintering aphid is controlled only by whitewashing.
Three goldenrain tree planting areas in the same area are selected as experimental areas, overwintering aphids are controlled according to the control means of the embodiment 3, the embodiment 4 and the comparative example 1, whether the aphid outbreak phenomenon occurs or not is observed in the next 4-5 months, and as a result, the aphid outbreak phenomenon does not occur in the experimental areas of the embodiment 3 and the embodiment 4 and occurs in the experimental area of the comparative example 1.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. A method for controlling overwintering aphids of goldenrain trees is characterized by comprising the following steps: the method comprises the following steps:
step one, ecological prevention and control;
applying biological compound fertilizer to the goldenrain tree in 9 months, controlling the application once every half month, and applying 10-12kg per mu;
secondly, physical prevention and control;
the method comprises the following steps of scraping old and beautiful barks of the trunk of the goldenrain tree in 10-11 months and whitewashing the trunk and backbone boughs of the goldenrain tree by using a whitewash agent;
thirdly, biological prevention and control;
suspending the ladybug phagostimulant at a position 3-5cm higher than an action target in the aphid group in the month of 4, wherein the distance between every two ladybug phagostimulants is 10cm, and releasing the seed ladybugs in the aphid group;
and fourthly, chemical prevention and treatment.
2. An aphid eliminating method for the overwintering of goldenrain tree as claimed in claim 1, wherein said biological compound fertilizer is prepared by mixing koffy, HYT-A strain agent and HYT-B strain agent according to the weight ratio of 1: 0.2-0.5: 0.3-0.5.
3. The method for eliminating overwintering aphids of goldenrain trees according to claim 1, characterized in that the ladybug phagostimulant is prepared by the following steps:
step S1, adding beta-cyclodextrin into deionized water, slowly dropwise adding a sodium hydroxide aqueous solution with the concentration of 8mol/L, and uniformly stirring after dropwise adding is finished until a system is clear to prepare a solution a; adding paratoluensulfonyl chloride into acetonitrile, and stirring at a constant speed until the mixture is dissolved to prepare a solution b; dropwise adding the solution b into the solution a, uniformly stirring at room temperature, reacting for 2 hours, carrying out suction filtration, removing filter residues, dropwise adding dilute hydrochloric acid with the mass fraction of 10% to adjust the pH until the pH is 6, and carrying out cold storage at 5 ℃ for 12 hours to obtain an intermediate 1;
step S2, adding the intermediate 1, sodium iodide and ethylenediamine into a flask, dropwise adding N-methyl pyrrolidone, completely adding the N-methyl pyrrolidone, introducing nitrogen, heating to 95 ℃, uniformly stirring and reacting for 5 hours, transferring the mixture into absolute ethyl alcohol after the reaction is finished, standing until precipitates are separated out, performing suction filtration to obtain a primary material, adding the primary material into deionized water, uniformly stirring and adding pheromone, continuously stirring for 15min, then adding hydroxyethyl cellulose, and performing ultrasonic treatment for 30min to obtain the ladybug phagostimulant.
4. The method for controlling overwintering aphids of goldenrain trees according to claim 3, characterized in that: the pheromone is formed by mixing trans-beta-farnesene and cis-3-hexenol according to the weight ratio of 2: 1.
5. The method for controlling overwintering aphids of goldenrain trees according to claim 3, characterized in that: in step S1, the dosage ratio of beta-cyclodextrin, sodium hydroxide aqueous solution and deionized water is controlled to be 60 g: 20 mL: 500mL, the dosage ratio of paratoluensulfonyl chloride and acetonitrile is controlled to be 10.05 g: 35mL, and the volume ratio of solution b to solution a is controlled to be 1: 12-15.
6. The method for controlling overwintering aphids of goldenrain trees according to claim 3, characterized in that: in step S2, the dosage ratio of the intermediate 1, the sodium iodide, the ethylenediamine and the N-methyl pyrrolidone is controlled to be 2.5 g: 0.015 g: 0.35 g: 5mL, and the dosage ratio of the initial material, the pheromone, the deionized water and the hydroxyethyl cellulose is controlled to be 0.25 g: 0.025 g: 5 mL: 0.4 g.
7. The method for controlling overwintering aphids of goldenrain trees according to claim 1, characterized in that: the chemical control comprises the following steps: the yellow mountain goldenrain tree is sprayed with the prevention and cure agent in 4-5 months of the year.
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