Preparation method and application of fluralan composite insecticide

Abstract

The invention relates to the technical field of pesticides, in particular to a preparation method and application of a fluralan composite insecticide, the preparation method comprises the following steps: firstly, uniformly mixing fluralan and spirotetramat, then adding the mixture into ethanol, uniformly stirring, then adding soybean oil, and uniformly stirring again to prepare a composite insecticidal solution; then, embedding the composite insecticidal liquid by using a combined liquid A prepared from a sodium tripolyphosphate solution, a glacial acetic acid solution, chitosan, sodium alginate and octylphenol polyoxyethylene ether, so as to prepare a microcapsule A; embedding the composite insecticidal liquid by using a combined liquid B prepared from N-hydroxysuccinimide, water, pectin and sodium methylene bis-naphthalene sulfonate, so as to prepare a microcapsule B; and finally, mixing the microcapsule A, the microcapsule B and the flurala according to a specific ratio to prepare the flurala composite insecticide which is high in environmental adaptability, can efficiently kill insects for a long time and has a wide application prospect.

Description

Technical Field

[0001] The invention relates to the technical field of pesticides, and in particular to a preparation method and application of a flurellan composite insecticide. Background Art

[0002] Fluorella is a new type of isoxazoline broad-spectrum insecticide that acts on γ-aminobutyric acid receptors. The original drug is a white or white crystalline powder with a melting point of 123-125°C and a boiling point of 314.4-384.4°C. It has low solubility in water and high solubility in organic solvents such as methanol, ethanol, acetone, ethyl acetate and dimethyl sulfoxide. The mechanism of action of Fluorella is to gate the chloride ion channels of glutamate and γ-aminobutyric acid receptors of invertebrates, preventing chloride ions from penetrating into the postsynaptic membrane, thereby interfering with the transmembrane signal transmission of the nervous system, causing disorders of the insect nervous system, and ultimately leading to the death of the insect. Fluorella not only exhibits high efficiency and low toxicity insecticidal activity against pests such as Lepidoptera, Hemiptera, Thysanoptera, and Acarina, but is also safe for non-target organisms such as mammals, zebrafish, and poultry, showing broad application prospects.

[0003] At present, flurellana has been widely used as a new type of antiparasitic veterinary drug. For example, patent technology document CN114306231B discloses a flurellana insecticide and its preparation method and application. The flurellana insecticide of the invention comprises flurellana, a cosolvent, a composite diluent and an organic solvent. A prescribed amount of flurellana is dissolved in an organic solvent; then the cosolvent and the composite diluent are added in sequence and mixed evenly to obtain the flurellana insecticide.

[0004] However, the research and development and promotion of flurellana as a pesticide is still in its infancy, and the existing technology only shows that flurellana has good insecticidal activity. It does not specifically explain how to use flurellana to prepare agricultural insecticides and solve the problem that flurellana insecticides cannot effectively kill insects in the long term.

[0005] Therefore, according to the above-mentioned related technologies, it is urgent to develop a preparation method of the flurellana composite insecticide. Summary of the invention

[0006] In view of this, the purpose of the present invention is to provide a method for preparing a flurellan compound insecticide, so as to provide a long-term and highly effective flurellan compound agricultural insecticide.

[0007] Based on the above purpose, the present invention provides a preparation method and application of a flurellan composite insecticide.

[0008] A method for preparing a flurellan composite insecticide comprises the following steps:

[0009] Step S1: adding the composite insecticide solution dropwise to the combined liquid A, stirring for the first time, then adding the sodium tripolyphosphate solution dropwise, stirring for the second time, centrifuging at high speed, washing the lower layer of sediment by centrifugation for 3-5 times, filtering and drying in sequence, to obtain microcapsules A;

[0010] Step S2: adding the composite insecticide solution dropwise to the combined solution B, stirring for the first time, then adding N-hydroxysuccinimide, stirring for the second time, centrifuging at high speed, washing the lower layer of sediment by centrifugation for 3-5 times, filtering and drying in sequence, to obtain microcapsules B;

[0011] Step S3: mixing microcapsule A, microcapsule B and flurella evenly to obtain a flurella composite insecticide;

[0012] The combined liquid A is prepared from glacial acetic acid solution, chitosan, sodium alginate and octylphenol polyoxyethylene ether in a mass ratio of 1000-1150:7-10:13-15:20-23;

[0013] The combined liquid B is prepared from water, pectin and sodium methylene bisnaphthalene sulfonate in a mass ratio of 1000-1050:8-9.5:20-23;

[0014] The composite insecticide solution is prepared from ethanol, flurellana, spirotetramat and soybean oil in a mass ratio of 7-10:2.3-3:1.7-2:17-20;

[0015] The mass ratio of the microcapsule A, microcapsule B and flurella is 30-33:17-20:0.0001-0.0002.

[0016] Preferably, the preparation method of the combined liquid A in step S1 is as follows:

[0017] Chitosan and sodium alginate are added to a 0.8%-1.1% glacial acetic acid solution, and the mixture is stirred at 25-30°C for 2-2.5 hours. The pH value is then adjusted to 4.2-4.5 with a 5%-8% sodium hydroxide solution, and octylphenol polyoxyethylene ether is added. The mixture is stirred at 20-30°C for 1-1.5 hours to obtain a combined liquid A.

[0018] Preferably, the preparation method of the combined liquid B in step S2 is as follows:

[0019] Pectin was added to water, and the mixture was stirred at 25-30°C for 2-2.5 hours. Then, sodium methylenebisnaphthalenesulfonate was added, and the mixture was stirred at 20-30°C for 1-1.5 hours to obtain a combined solution B.

[0020] Preferably, the preparation method of the composite insecticide liquid is as follows:

[0021] After mixing flurellana and spirotetramat evenly, add them into ethanol, stir evenly, add soybean oil, stir evenly again, and obtain a composite insecticide solution.

[0022] Preferably, the mass ratio of the combined liquid A, the composite insecticide liquid and the sodium tripolyphosphate solution in step S1 is 1050-1200:17-20:300-350.

[0023] Preferably, in step S2, the mass ratio of the combined liquid B, the composite insecticide liquid and N-hydroxysuccinimide is 1050-1200:10-11.5:30-35.

[0024] Preferably, the concentration of the sodium tripolyphosphate solution in step S1 is 4.7%-5.0%.

[0025] Preferably, in step S1, the temperature during the first stirring is 25-30°C, and the stirring time is 1-1.3h; the temperature during the second stirring is 25-28°C, and the stirring time is 2-2.5h; the speed during the high-speed centrifugation is 10000-11000r / min, and the centrifugation time is 30-35min; the pore size of the filter paper during the filtration is 0.40-0.45μm; the temperature during the drying treatment is 28-30°C, and the time is 47-50h.

[0026] Preferably, in step S2, the temperature during the first stirring is 25-30°C, and the stirring time is 1-1.3h; the temperature during the second stirring is 25-28°C, and the stirring time is 2-2.5h; the speed during the high-speed centrifugation is 10000-11000r / min, and the centrifugation time is 30-35min; the pore size of the filter paper during the filtration is 0.45-0.50μm; the temperature during the drying treatment is 55-60°C, and the time is 12-15h.

[0027] The invention discloses an application of a flurellana compound insecticide, wherein the flurellana compound insecticide is used for killing common pests in the growth process of crops.

[0028] Beneficial effects of the present invention:

[0029] The present invention provides a preparation method and application of a flurellaner composite insecticide. Firstly, the present invention effectively improves the insecticidal activity and action range of the insecticide by compounding flurellaner with spirotetramat and dissolving the compound in ethanol and soybean oil, prevents flurellaner from being reacted by hypochlorous acid in water, and alleviates the problem of extremely low solubility of flurellaner in water.

[0030] Secondly, the present invention mixes microcapsules A, microcapsules B and flurella in a specific ratio, so that the prepared flurella compound insecticide can kill insects immediately and effectively for a long time;

[0031] Moreover, one of the two different dispersants used in the two microcapsules of the present invention is a nonionic dispersant and the other is an anionic dispersant. When the two dispersants meet, they will interact with each other and further disperse the composite insecticide liquid, thereby further enhancing the insecticidal activity of the insecticide.

[0032] Therefore, compared with the prior art, the flurellanine compound insecticide prepared by the present invention has higher stability, insecticidal activity, timeliness and wider application prospects. DETAILED DESCRIPTION

[0033] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0034] The sources and properties of some of the raw materials used in the present invention are as follows:

[0035] Flurellana was purchased from Shandong Chenghui Pharmaceutical Group Co., Ltd., CAS: 864731-61-3; spirotetramat was purchased from Hebei Xingbai Agricultural Science and Technology Co., Ltd., CAS: 203313-25-1; octylphenol polyoxyethylene ether was purchased from Shandong Yonglida New Materials Technology Co., Ltd., CAS: 9036-19-5; sodium methylene bisnaphthalene sulfonate was purchased from Wuhan Kanos Technology Co., Ltd., CAS: 36290-04-7; N-hydroxysuccinimide was purchased from Wuhan Xinzhongke Chemical Technology Co., Ltd., CAS: 6066-82-6.

[0036] Example 1: A method for preparing a flurellan composite insecticide.

[0037] S1: 2.4 g of flurellana and 1.7 g of spirotetramat were mixed evenly, added to 7 g of ethanol, stirred evenly, and then 17 g of soybean oil was added, and stirred evenly again to obtain a composite insecticide solution;

[0038] S2: Add 7 g of chitosan and 13 g of sodium alginate to 1000 g of 0.8% glacial acetic acid solution, stir at 25° C. for 2 h, then adjust the pH value to 4.2 with 5% sodium hydroxide solution, add 20 g of octylphenol polyoxyethylene ether, and stir at 20° C. for 1 h to obtain a combined solution A;

[0039] S3: adding 8 g of pectin to 1000 g of water, stirring at 25° C. for 2 h, then adding 20 g of sodium methylene bisnaphthalene sulfonate, stirring at 20° C. for 1 h, to obtain a combined solution B;

[0040] S4: 17 g of the composite insecticide was added dropwise to 1050 g of the combined liquid A, and the mixture was stirred at 25° C. for 1 h. Then, 300 g of a 4.7% sodium tripolyphosphate solution was added dropwise, and the mixture was stirred at 25° C. for 2 h. After high-speed centrifugation at 10,000 r / min for 30 min, the lower sediment was centrifuged and washed three times, and then filtered with a filter paper with a pore size of 0.40 μm, and then dried at 28° C. for 47 h to obtain microcapsules A;

[0041] S5: 10 g of the composite insecticide solution was added dropwise to 1050 g of the combined liquid B, and the mixture was stirred at 25°C for 1 h. Then, 30 g of N-hydroxysuccinimide was added, and the mixture was stirred at 25°C for 2 h. After high-speed centrifugation at 10,000 r / min for 30 min, the lower sediment was centrifuged and washed three times, and then filtered with a filter paper with a pore size of 0.45 μm, and then dried at 55°C for 12 h to obtain microcapsules B;

[0042] S6: 30 g of microcapsule A, 17 g of microcapsule B and 0.0001 g of flurella are mixed evenly to obtain a flurella compound insecticide.

[0043] Example 2: A method for preparing a flurellan composite insecticide.

[0044] S1: 2.6 g of flurellana and 1.8 g of spirotetramat were mixed evenly, added to 8 g of ethanol, stirred evenly, and then 18 g of soybean oil was added, and stirred evenly again to obtain a composite insecticide solution;

[0045] S2: Add 8 g of chitosan and 13.5 g of sodium alginate to 1050 g of 0.9% glacial acetic acid solution, stir at 27° C. for 2.2 h, then adjust the pH value to 4.3 with 6% sodium hydroxide solution, add 21 g of octylphenol polyoxyethylene ether, and stir at 23° C. for 1.2 h to obtain a combined solution A;

[0046] S3: Add 8.5 g of pectin to 1020 g of water, stir at 27° C. for 2.2 h, then add 21 g of sodium methylene bisnaphthalene sulfonate, stir at 23° C. for 1.2 h, to obtain a combined solution B;

[0047] S4: 18 g of the composite insecticide solution was added dropwise to 1100 g of the combined liquid A, and the mixture was stirred at 27° C. for 1.1 h, and then 320 g of a 4.8% sodium tripolyphosphate solution was added dropwise, and the mixture was stirred at 26° C. for 2.2 h. After high-speed centrifugation at 10300 r / min for 32 min, the lower sediment was centrifuged and washed 4 times, and then filtered with a filter paper with a pore size of 0.42 μm, and then dried at 29° C. for 48 h to obtain microcapsules A;

[0048] S5: 10.5 g of the composite insecticide was added dropwise to 1100 g of the combined liquid B, and the mixture was stirred at 27° C. for 1.1 h, followed by the addition of 32 g of N-hydroxysuccinimide, and the mixture was stirred at 26° C. for 2.2 h. The lower precipitate was centrifuged and washed 4 times at a high speed of 10300 r / min for 32 min, and then filtered with a filter paper with a pore size of 0.47 μm, and then dried at 57° C. for 13 h to obtain microcapsules B;

[0049] S6: 31 g of microcapsule A, 18 g of microcapsule B and 0.00013 g of flurella are mixed evenly to obtain a flurella compound insecticide.

[0050] Example 3: A method for preparing a flurellan composite insecticide.

[0051] S1: 2.8 g of flurellana and 1.9 g of spirotetramat were mixed evenly, added to 9 g of ethanol, stirred evenly, and then 19 g of soybean oil was added, and stirred evenly again to obtain a composite insecticide solution;

[0052] S2: Add 9 g of chitosan and 14.5 g of sodium alginate to 1100 g of 1.0% glacial acetic acid solution, stir at 29° C. for 2.4 h, then adjust the pH value to 4.4 with 7% sodium hydroxide solution, add 22 g of octylphenol polyoxyethylene ether, and stir at 27° C. for 1.4 h to obtain a combined solution A;

[0053] S3: Add 9 g of pectin to 1040 g of water, stir at 29° C. for 2.4 h, then add 22 g of sodium methylene bis-naphthalene sulfonate, and stir at 27° C. for 1.4 h to obtain a combined solution B;

[0054] S4: 19 g of the composite insecticide solution was added dropwise to 1150 g of the combined liquid A, and the mixture was stirred at 29° C. for 1.2 h. Then, 340 g of a 4.9% sodium tripolyphosphate solution was added dropwise, and the mixture was stirred at 27° C. for 2.4 h. After high-speed centrifugation at 10700 r / min for 34 min, the lower sediment was centrifuged and washed 4 times, and then filtered with a filter paper with a pore size of 0.44 μm, and then dried at 29° C. for 49 h to obtain microcapsules A;

[0055] S5: 11 g of the composite insecticide was added dropwise to 1150 g of the combined liquid B, and the mixture was stirred at 29°C for 1.2 h. Then, 34 g of N-hydroxysuccinimide was added, and the mixture was stirred at 27°C for 2.4 h. After high-speed centrifugation at 10700 r / min for 34 min, the lower sediment was centrifuged and washed 4 times, and then filtered with a filter paper with a pore size of 0.49 μm, and then dried at 59°C for 14 h to obtain microcapsules B;

[0056] S6: 32 g of microcapsule A, 19 g of microcapsule B and 0.00017 g of flurella are mixed uniformly to obtain a flurella composite insecticide.

[0057] Example 4: A method for preparing a flurellan composite insecticide.

[0058] S1: 3g of flurellana and 2g of spirotetramat were mixed evenly, then added to 10g of ethanol, stirred evenly, and then 20g of soybean oil was added, and stirred evenly again to obtain a composite insecticide solution;

[0059] S2: Add 10 g of chitosan and 15 g of sodium alginate to 1150 g of 1.1% glacial acetic acid solution, stir at 30° C. for 2.5 h, then adjust the pH value to 4.5 with 8% sodium hydroxide solution, add 23 g of octylphenol polyoxyethylene ether, and stir at 30° C. for 1.5 h to obtain a combined solution A;

[0060] S3: Add 9.5 g of pectin to 1050 g of water, stir at 30° C. for 2.5 h, then add 23 g of sodium methylene bisnaphthalene sulfonate, stir at 30° C. for 1.5 h, to obtain a combined solution B;

[0061] S4: 20 g of the composite insecticide solution was added dropwise to 1200 g of the combined liquid A, and the mixture was stirred at 30° C. for 1.3 h. Then, 350 g of a 5.0% sodium tripolyphosphate solution was added dropwise, and the mixture was stirred at 28° C. for 2.5 h. After high-speed centrifugation at 11000 r / min for 35 min, the lower sediment was centrifuged and washed 5 times, and then filtered with a filter paper with a pore size of 0.45 μm, and then dried at 30° C. for 50 h to obtain microcapsules A;

[0062] S5: 11.5 g of the composite insecticide was added dropwise to 1200 g of the combined liquid B, and the mixture was stirred at 30° C. for 1.3 h, followed by the addition of 35 g of N-hydroxysuccinimide, and the mixture was stirred at 28° C. for 2.5 h. The lower precipitate was centrifuged and washed five times at a high speed of 11000 r / min for 35 min, and then filtered with a filter paper having a pore size of 0.50 μm, and then dried at 60° C. for 15 h to obtain microcapsules B;

[0063] S6: 33 g of microcapsule A, 20 g of microcapsule B and 0.0002 g of flurella are mixed evenly to obtain a flurella compound insecticide.

[0064] Comparative Example 1:

[0065] Compared with Example 1, this comparative example did not add spirotetramat during the preparation of the composite insecticide solution, and the remaining steps and parameters were the same, which will not be repeated in this comparative example, and finally the flurellana composite insecticide was obtained.

[0066] Comparative Example 2:

[0067] Compared with Example 1, this comparative example only replaces "0.45 μm" with "0.40 μm", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally the flurellan composite insecticide is obtained.

[0068] Comparative Example 3:

[0069] Compared with Example 1, this comparative example only replaces "30g microcapsule A, 17g microcapsule B and 0.0001g flurella" with "23.5g microcapsule A, 23.5g microcapsule B and 0.0001g flurella", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally the flurella composite insecticide is obtained.

[0070] Comparative Example 4:

[0071] Compared with Example 1, this comparative example only replaces "3.0g microcapsule A, 1.7g microcapsule B and 0.0001g flurella" with "3.0g microcapsule A and 1.7g microcapsule B", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally the flurella compound insecticide is obtained.

[0072] Comparative Example 5: A method for preparing a flurellan composite insecticide.

[0073] S1: 2.4 g of flurellana and 2 g of spirotetramat were mixed evenly, added to 10 g of ethanol, stirred evenly, and then 20 g of soybean oil was added, and stirred evenly again to obtain a composite insecticide solution;

[0074] S2: Add 14 g of chitosan and 26 g of sodium alginate to 2000 g of 0.8% glacial acetic acid solution, stir at 25° C. for 2 h, then adjust the pH value to 4.2 with 5% sodium hydroxide solution, add 40 g of octylphenol polyoxyethylene ether, and stir at 20° C. for 1 h to obtain a combined solution A;

[0075] S3: 17 g of the composite insecticide was added dropwise to 1050 g of the combined liquid A, and the mixture was stirred at 25° C. for 1 h. Then, 300 g of a 4.7% sodium tripolyphosphate solution was added dropwise, and the mixture was stirred at 25° C. for 2 h. After high-speed centrifugation at 10,000 r / min for 30 min, the lower sediment was centrifuged and washed three times, and then filtered with a filter paper with a pore size of 0.40 μm, and then dried at 28° C. for 47 h to obtain microcapsules A;

[0076] S4: 47 g of microcapsule A and 0.0001 g of flurella are mixed evenly to obtain a flurella compound insecticide.

[0077] Comparative Example 6: A method for preparing a flurellan composite insecticide.

[0078] S1: 2.4 g of flurellana and 1.7 g of spirotetramat were mixed evenly, added to 7 g of ethanol, stirred evenly, and then 17 g of soybean oil was added, and stirred evenly again to obtain a composite insecticide solution;

[0079] S2: Add 24 g of pectin to 3000 g of water, stir at 25° C. for 2 h, then add 60 g of sodium methylene bisnaphthalene sulfonate, stir at 20° C. for 1 h, to obtain a combined solution B;

[0080] S3: 34.5 g of the composite insecticide was added dropwise to 3060 g of the combined liquid B, and the mixture was stirred at 25°C for 1 h. Then, 105 g of N-hydroxysuccinimide was added, and the mixture was stirred at 25°C for 2 h. After high-speed centrifugation at 10,000 r / min for 30 min, the lower sediment was centrifuged and washed three times, and then filtered with a filter paper with a pore size of 0.45 μm, and then dried at 55°C for 12 h to obtain microcapsules B;

[0081] S4: 47 g of microcapsule B and 0.0001 g of flurella are mixed evenly to obtain a flurella compound insecticide.

[0082] Comparative Example 7: A method for preparing a flurellan composite insecticide.

[0083] S1: 2.4 g of flurellana and 1.7 g of spirotetramat were mixed evenly, added to 7 g of ethanol, stirred evenly, and then 17 g of soybean oil was added, and stirred evenly again to obtain a composite insecticide solution;

[0084] S2: Add 0.5 g of octylphenol polyoxyethylene ether to 27 g of the composite insecticide solution, and stir at 20° C. for 1 h to obtain a flurellan composite insecticide.

[0085] Performance Test:

[0086] The flurellana composite insecticides prepared in Examples 1 to 4 and Comparative Examples 1 to 7 were diluted with 500 mL of water to obtain insecticides, and the performance of the obtained insecticides was tested:

[0087] Testing of soil pH changes:

[0088] Referring to the test standard NY / T1121.2-2006 "Soil Testing. Part 2: Determination of Soil pH", weigh 10g of air-dried soil that has passed through a 2mm aperture sieve, add 25mL of water that has been degassed with CO2, stir until the soil particles are fully dispersed, and after standing for 30 minutes, insert the electrode into the sample suspension, let it stand for a while, press the reading switch, and record the pH value when the reading stabilizes. The same method was used to test the pH value of the homologous soil 60 days after spraying the pesticide. After measuring every 5-6 samples, the standard solution should be used to check the positioning. According to this method, the soil pH change value of the insecticide diluted from the flurellana composite insecticide of Examples 1-4 and Comparative Examples 1-7 was determined. Among them, the soil pH change value is the difference between the pH value of the soil without pesticide spraying and the pH value of the soil sprayed with pesticide; the test results are shown in Table 1;

[0089] Test for reduction of mercury content in soil:

[0090] According to the test standard of GB / T22105.1-2008 "Soil quality - determination of total mercury, total arsenic and total lead - atomic fluorescence method. Part 1: determination of total mercury in soil", 1.0g of the air-dried, ground and 0.149mm sieve soil sample was weighed into a 50mL stoppered colorimetric tube, a little water was added to moisten the sample, 10mL of aqua regia was added, the stopper was added, and the sample was digested in a boiling water bath for 2h, the sample was taken out and cooled, 10mL of preservation solution was immediately added, the sample was diluted to the scale with diluent, the sample was placed after shaking, and the supernatant was taken to measure the fluorescence intensity under the conditions of pressure of 280V and temperature of 200℃, and a blank test was performed at the same time. Then the fluorescence intensity of the insecticide diluted by spraying the flurellana compound insecticide prepared in Examples 1 to 4 and Comparative Examples 1 to 7 was measured according to this method; wherein, the reduction value of soil mercury content (mg·kg -1 ) is the mercury content value in the soil sprayed with pesticides and the mercury content value in the soil not sprayed with pesticides; the test results are shown in Table 1;

[0091] Test of insecticidal rate at different times:

[0092] Refer to the test standard of NY / T1154.1-2006 "Guidelines for Indoor Bioassay Tests of Pesticides. Insecticides. Part 1: Contact Activity Test. Spot Method". When the room temperature is 25℃ and the air humidity is about 50%, use a brush to select a group of test insects between the ages of 3-4 and place them in a culture dish for use. The test insects in the culture dish are treated with drops one by one. Lepidoptera larvae are dripped on the pronotum of the insect body, and 0.5μL-1.0μL of insecticide is dripped on each head; aphids, planthoppers, etc. are dripped on the abdomen of the insect body, and 0.02μL-0.1μL of insecticide is dripped on each head. The test insects after dripping are transferred to normal conditions for breeding. And 1L of water without pesticide is set as a control. Investigate the death of the test insects 24 hours after treatment, and record the total number of insects and the number of dead insects. The group of test insects includes 20 armyworms, 20 striped stem borers, 20 cotton bollworms, 20 aphids and 20 gray leafhoppers. The insecticide rate (%) of the diluted insecticide of the flurellana composite insecticide of Examples 1 to 4 and Comparative Examples 1 to 7 and the insecticide rate (%) of the diluted insecticide after being placed for 30 days are measured according to this method; the test results are shown in Table 1;

[0093] Insecticide rate calculation formula:

[0094] Test of insecticidal activity at different temperatures:

[0095] Referring to the test standard of NY / T1154.1-2006 "Guidelines for Indoor Bioassay Tests of Pesticides. Insecticides. Part 1: Contact Activity Test. Spot Method", when the air humidity is about 50%, a group of test insects between the ages of 3-4 are selected with a brush and placed in a culture dish for use. The test insects in the culture dish are treated with drops one by one. Lepidoptera larvae are dripped on the pronotum of the insect body, and 0.5μL-1.0μL of insecticide is dripped on each head; aphids, planthoppers, etc. are dripped on the abdomen of the insect body, and 0.02μL-0.1μL of insecticide is dripped on each head. The test insects after dripping are transferred to normal conditions for breeding. A group of 1L water without the agent is set as a control. The death of the test insects is investigated 24h after treatment, and the total number of insects and the number of dead insects are recorded. The group of test insects includes 20 sticky insects, 20 striped stem borers, 20 cotton bollworms, 20 aphids and 20 gray leafhoppers. According to this method, the insecticidal rates (%) of the diluted insecticides of the flurellana composite insecticides prepared in Examples 1 to 4 and Comparative Examples 1 to 7 at temperatures of 0°C and 50°C were measured respectively; the test results are shown in Table 1;

[0096] Insecticide rate calculation formula:

[0097] Test of insecticidal activity at different humidity:

[0098] Referring to the test standard of NY / T1154.1-2006 "Guidelines for Indoor Bioassay Tests of Pesticides. Insecticides. Part 1: Contact Activity Test. Spot Method", at room temperature of about 25°C, a group of test insects between the ages of 3 and 4 were selected with a brush and placed in a culture dish for use. The test insects in the culture dish were treated with drops one by one, and the lepidopteran larvae were dripped on the pronotum of the insect body, and 0.5μL-1.0μL of insecticide was dripped on each head; aphids, planthoppers, etc. were dripped on the abdomen of the insect body, and 0.02μL-0.1μL of insecticide was dripped on each head. The test insects after dripping were transferred to normal conditions for breeding. A group of 1L water without the agent was set as a control. The death of the test insects was investigated 24 hours after treatment, and the total number of insects and the number of dead insects were recorded. The group of test insects included 20 sticky insects, 20 striped stem borers, 20 cotton bollworms, 20 aphids and 20 gray leafhoppers. According to this method, the insecticidal rates (%) of the diluted insecticides of the flurellana composite insecticides prepared in Examples 1 to 4 and Comparative Examples 1 to 7 at humidity of 20% and 90% were measured respectively; the test results are shown in Table 1;

[0099] Insecticide rate calculation formula:

[0100] Table 1

[0101]

[0102]

[0103] Data Analysis:

[0104] It can be seen from Table 1 that the flurellana composite insecticide prepared by the present invention has stronger ability to adjust soil pH, reduce soil mercury content, long-acting insecticide ability, high and low temperature resistance, and dry and wet resistance, that is, the flurellana composite insecticide prepared by the present invention has stronger soil recovery ability, insecticidal ability, long-acting insecticidal ability and environmental adaptability.

[0105] This may be because, by compounding flurana with spirotetramat and dissolving them in ethanol and soybean oil, the present invention effectively improves the insecticidal activity, insecticidal range and insecticidal time of the insecticide, prevents flurana from being reacted by hypochlorous acid in water, and alleviates the problem of extremely low solubility of flurana in water; secondly, the decomposition time of microcapsule A in the two microcapsules prepared by the present invention is about 3h-10d, and the decomposition time of microcapsule B is about 6h-45d. The present invention mixes these two types of microcapsules with flurana, so that the prepared flurana composite insecticide can not only kill insects immediately, but also can be used for a long time. Time-efficient insecticide; moreover, among the two different dispersants used in the two microcapsules of the present invention, one is a nonionic dispersant and the other is an anionic dispersant. When the two dispersants meet, they interact with each other and further disperse the composite insecticide liquid, thereby further enhancing the insecticidal activity of the insecticide; in addition, the microcapsule shell material used in the present invention has good heavy metal adsorption capacity and stability, and the core material has good pH adjustment ability. Therefore, the flurellana composite insecticide prepared by the present invention has stronger soil recovery ability, insecticidal ability, long-acting insecticidal ability and environmental adaptability.

[0106] In Comparative Example 1, spirotetramat was not added during the preparation of the composite insecticide. It can be seen from Table 1 that compared with the insecticide prepared in Example 1, the insecticidal rate in various cases decreased. This may be because the compound use of spirotetramat and flurellan can effectively improve the insecticidal activity of the insecticide. In Comparative Example 2, "0.45 μm" was replaced by "0.40 μm". It can be seen from Table 1 that compared with the insecticide prepared in Example 1, the insecticidal rate in various cases decreased, among which the insecticidal rate decreased the most after 30 days. This may be because the original microcapsule B was a particle with a particle size of no more than 0.45 μm, with more core material and thicker capsule. When the particle size is reduced to no more than 0.40 μm, not only the core material content of microcapsule B is reduced, but also the thickness of the capsule shell is thinner, so the decomposition time of microcapsule B is reduced, and the insecticide rate is significantly reduced after 30 days; in Comparative Example 3, "30 g microcapsule A, 17 g microcapsule B and 0.0001 g flurella" is replaced by "23.5 g microcapsule A, 23.5 g microcapsule B and 0.0001 g flurella", and it can be seen from Table 1 that compared with the insecticide prepared in Example 1, its ability to reduce soil pH and mercury content is reduced, and the insecticide rate in various cases is also reduced. This may be due to the fact that microcapsule A has higher acidity and heavy metal absorption than microcapsule B. The content of microcapsule A in this comparative example is reduced, while the content of microcapsule B is increased, which will lead to a later overall decomposition time of the insecticide, resulting in a decrease in the ability of the newly prepared insecticide to reduce soil pH and mercury content, and a relatively low insecticide rate; in comparative example 4, "30g microcapsule A, 17g microcapsule B and 0.0001g flurella" is replaced by "30g microcapsule A and 17g microcapsule B". It can be seen from Table 1 that compared with the insecticide prepared in Example 1, the insecticide rate in various cases has decreased. This may be because the absence of direct addition of flurella will reduce the active ingredient of the insecticide, and the direct addition of more soluble Flurella, although part of Flurella will not dissolve, it will also be dispersed in the system, and play a rapid insecticidal effect before the microcapsules decompose; Comparative Example 5 did not prepare and add microcapsules A, but directly compounded 47g of microcapsules B with 0.0001g of Flurella to prepare Flurella composite insecticide. It can be seen from Table 1 that compared with the insecticide prepared in Example 1, its ability to reduce soil pH and mercury content decreased, and the insecticidal rate in various cases also decreased. This may be because microcapsules A have higher acidity, heavy metal adsorption capacity and shorter decomposition time than microcapsules B; Comparative Example 6 did not prepare and add microcapsules B, but directly compounded 47g of microcapsules A with 0.0001g of Flurella.0001g of flurellana was compounded to prepare a flurellana composite insecticide. It can be seen from Table 1 that compared with the insecticide prepared in Example 1, its ability to reduce soil pH and mercury content was slightly improved, and the insecticide rate in various cases decreased, among which the insecticide rate decrease rate after 30 days was particularly prominent. This may be because the decomposition time of microcapsule A is shorter than that of microcapsule B. Microcapsule A has been basically completely decomposed before 30 days, but it still has a certain insecticide ability because after the decomposition of microcapsule A, part of the flurellana and spirotetramat in the core material are still protected by soybean oil and will not be reacted by the active substances in water; Comparative Example 7 did not prepare and add microcapsules A and microcapsules B, but directly used the original composite insecticide in Example 1 as the flurellana composite insecticide. Therefore, it can be seen from Table 1 that compared with the insecticide prepared in Example 1, it can basically no longer reduce the soil pH and mercury content, and the insecticide rate in various cases has also decreased, among which the insecticide rate decrease rate after 30 days is particularly prominent. This may be because the microcapsules used in the present invention have a certain acidity, heavy metal adsorption capacity, stability and slow release capacity, which can allow the prepared insecticide to adapt well to environmental changes while also being able to kill insects and repair soil in a long-term and efficient manner. .

[0107] Those skilled in the art should understand that the discussion of any of the above embodiments is merely illustrative and is not intended to imply that the scope of the present invention is limited to these examples. Under the concept of the present invention, the technical features in the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity.

[0108] The present invention is intended to cover all such substitutions, modifications and variations that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A method for preparing a flurellan composite insecticide, characterized in that: The specific steps include: Step S1: adding the composite insecticide solution dropwise to the combined liquid A, stirring for the first time, then adding the sodium tripolyphosphate solution dropwise, stirring for the second time, centrifuging at high speed, washing the lower layer of sediment by centrifugation for 3-5 times, filtering and drying in sequence, to obtain microcapsules A; Step S2: adding the composite insecticide solution dropwise to the combined solution B, stirring for the first time, then adding N-hydroxysuccinimide, stirring for the second time, centrifuging at high speed, washing the lower layer of sediment by centrifugation for 3-5 times, filtering and drying in sequence, to obtain microcapsules B; Step S3: mixing microcapsule A, microcapsule B and flurella evenly to obtain a flurella compound insecticide; The combined liquid A is prepared from glacial acetic acid solution, chitosan, sodium alginate and octylphenol polyoxyethylene ether in a mass ratio of 1000-1150:7-10:13-15:20-23; The combined liquid B is prepared from water, pectin and sodium methylene bisnaphthalene sulfonate in a mass ratio of 1000-1050:8-9.5:20-23; The composite insecticide solution is prepared from ethanol, flurellana, spirotetramat and soybean oil in a mass ratio of 7-10:2.4-3:1.7-2:17-20; The mass ratio of the microcapsule A, microcapsule B and flurella is 30-33:17-20:0.0001-0.0002.

2. The method for preparing the fluororana composite insecticide according to claim 1, characterized in that: The preparation method of the combined liquid A in step S1 is as follows: Chitosan and sodium alginate are added to a 0.8%-1.1% glacial acetic acid solution, and the mixture is stirred at 25-30°C for 2-2.5 hours. The pH value is then adjusted to 4.2-4.5 with a 5%-8% sodium hydroxide solution, and octylphenol polyoxyethylene ether is added. The mixture is stirred at 20-30°C for 1-1.5 hours to obtain a combined liquid A.

3. The method for preparing the fluororana composite insecticide according to claim 1, characterized in that: The preparation method of the combined liquid B in step S2 is as follows: Pectin was added to water, and the mixture was stirred at 25-30°C for 2-2.5 hours. Then, sodium methylenebisnaphthalenesulfonate was added, and the mixture was stirred at 20-30°C for 1-1.5 hours to obtain a combined solution B.

4. The method for preparing the fluororana composite insecticide according to claim 1, characterized in that: The preparation method of the composite insecticide liquid is as follows: After mixing flurellana and spirotetramat evenly, add them into ethanol, stir evenly, add soybean oil, stir evenly again, and obtain a composite insecticide solution.

5. The method for preparing the fluororana composite insecticide according to claim 1, characterized in that: The mass ratio of the combined liquid A, the composite insecticide liquid and the sodium tripolyphosphate solution in step S1 is 1050-1200:17-20:300-350.

6. The method for preparing the fluororana composite insecticide according to claim 1, characterized in that: The mass ratio of the combined liquid B, the compound insecticide liquid and N-hydroxysuccinimide in step S2 is 1050-1200:10-11.5:30-35.

7. The method for preparing the fluororana composite insecticide according to claim 1, characterized in that: The concentration of the sodium tripolyphosphate solution in step S1 is 4.7%-5.0%.

8. The method for preparing the fluororana composite insecticide according to claim 1, characterized in that: In step S1, the temperature during the first stirring is 25-30°C, and the stirring time is 1-1.3h; the temperature during the second stirring is 25-28°C, and the stirring time is 2-2.5h; the rotation speed during the high-speed centrifugation is 10000-11000r / min, and the centrifugation time is 30-35min; the pore size of the filter paper during the filtration is 0.40-0.45μm; the temperature during the drying treatment is 28-30°C, and the time is 47-50h.

9. The method for preparing the fluororana composite insecticide according to claim 1, characterized in that: In step S2, the temperature during the first stirring is 25-30°C, and the stirring time is 1-1.3h; the temperature during the second stirring is 25-28°C, and the stirring time is 2-2.5h; the speed during the high-speed centrifugation is 10000-11000r / min, and the centrifugation time is 30-35min; the pore size of the filter paper during the filtration is 0.45-0.50μm; the temperature during the drying treatment is 55-60°C, and the time is 12-15h.

10. A use of the flurellana composite insecticide according to any one of claims 1 to 9, characterized in that: The flurellana compound insecticide is used to kill common pests in the growth process of crops.

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