CN117814247A - Pesticide granule for preventing and killing duckweed in lotus root field and preparation method thereof - Google Patents

Pesticide granule for preventing and killing duckweed in lotus root field and preparation method thereof Download PDF

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Publication number
CN117814247A
CN117814247A CN202311555128.XA CN202311555128A CN117814247A CN 117814247 A CN117814247 A CN 117814247A CN 202311555128 A CN202311555128 A CN 202311555128A CN 117814247 A CN117814247 A CN 117814247A
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granule
duckweed
lotus root
composite
preventing
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Inventor
邵宇
陈涛
祁月月
方国江
徐雅飞
卓家雄
金鑫雷
张平
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Zhejiang Tianfeng Biological Science Co ltd
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Zhejiang Tianfeng Biological Science Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/661,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms
    • A01N43/681,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms with two or three nitrogen atoms directly attached to ring carbon atoms
    • A01N43/70Diamino—1,3,5—triazines with only one oxygen, sulfur or halogen atom or only one cyano, thiocyano (—SCN), cyanato (—OCN) or azido (—N3) group directly attached to a ring carbon atom
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/26Biocides, 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 in coated particulate form
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/30Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01PBIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P13/00Herbicides; Algicides
    • A01P13/02Herbicides; Algicides selective
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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

Abstract

The embodiment of the invention discloses pesticide granules for preventing and killing duckweed in lotus root fields and a preparation method thereof. The pesticide granule comprises the following components in percentage by weight: 2-6% of prometryn, 0.75-2.25% of clomazone, 0.1-0.3% of penoxsulam, 1-3% of a composite emulsifier, 2-5% of a composite film forming agent, 1-3% of a solvent and the balance of a composite carrier. The granule provided by the invention can float on the water surface, active ingredients can be slowly released, the lotus root Tian Fuping can be well prevented and removed, the lotus root granule is highly safe to the lotus root, the problems of short lasting period, poor duckweed prevention effect on a deep lotus root field, easiness in generation of phytotoxicity and the like of the existing medicament in preventing and removing the lotus root Tian Fuping can be solved, and the lotus root granule has very high market value.

Description

Pesticide granule for preventing and killing duckweed in lotus root field and preparation method thereof
Technical Field
The embodiment of the invention relates to the technical field of pesticides, in particular to a pesticide granule for preventing and killing duckweed in lotus root fields and a preparation method thereof.
Background
The pesticide granule is a common pesticide dosage form, and the processing forms comprise an extrusion granulation method, a roller granulation method, a disc granulation method, an adsorption granulation method, a crushing granulation method and the like. Most of the application forms of the granules are direct broadcast application, and the effective components in the granules achieve the purpose of preventing and controlling targets through diffusion.
Duckweed (Lemna minor l.) belongs to the phylum angiosperm, magnales, alismatis, arisceae, duckweed, phyllosoma symmetry, green surface, pale yellow back, green white or purple, approximately circular, inverted oval or inverted oval. The water is distributed in each of the north and south provinces, and is used in paddy fields, pond biogas or other still water areas to form floating communities densely distributed on the water surface, and the breeding is fast, so that the water is like a plum blossom cloud: the leaf number is the number of leaves grown after one leaf is grown, and the leaf number is usually dominant in communities, so that the control difficulty is very difficult.
Duckweed can influence the air permeability of water, so that the water is insufficient in nutrient supply, and the respiration of aquatic organisms is influenced; and the duckweed can influence the transmittance of the water body, so that the photosynthesis of plants in the water is influenced.
The common pesticide formulation for preventing and treating duckweed at present comprises suspending agents, granules, emulsifiable concentrates, wettable powder, microemulsion and the like, and the application method is direct broadcasting or water spray.
The patent CN201410178951.8 weeding composition describes that clomazone, metolachlor and prometryn are compounded, and the composition is prepared into granules and water dispersible granules, and can be used for preventing and killing weeds such as lotus root Tian Fuping, barnyard grass, spirogyra, crabgrass and the like. Patent CN201510366265.8 discloses a herbicidal composition containing dicamba and fluroxypyr, which is prepared into wettable powder, water dispersible granule, suspending agent, microemulsion, oil, suspending agent and the like, and is used for controlling duckweed plants.
However, since duckweed grows on the surface of water, when we apply conventional pesticide formulations, the pesticide active ingredient will typically diffuse throughout the water. Through a large number of field applications, the pesticide can have good control effect on duckweed when the water layer in the area where the duckweed is located is smaller than 0.5 meter, but the control effect of the pesticide on the duckweed is obviously reduced along with the increase of the depth of the water when the water layer in the area where the duckweed is located is larger than 0.5 meter. The pesticide is applied to water, and the active pesticide component in the water is diluted by water along with the increase of the water layer, so that the concentration of the active pesticide component in the water cannot reach the lethal concentration of duckweed, and the solid particles of the active pesticide component dispersed in the water are settled to the soil surface layer at the bottom of the water under the action of gravity, thereby losing the prevention and control effect on the duckweed.
Disclosure of Invention
The invention provides a pesticide granule for preventing and killing duckweed in lotus root fields, which comprises prometryn, clomazone and penoxsulam as active ingredients, and is prepared by selecting an emulsifier, a film forming agent and a carrier according to a proper proportion and using a pan granulator. The duration of the prevention and treatment of duckweed is greatly prolonged, so that the times of pesticide use by farmers can be reduced, the cost of pesticide use is reduced, and the pollution of pesticides to the environment is reduced.
In order to achieve the above object, the embodiment of the present invention provides the following technical solutions:
according to a first aspect of the embodiment of the invention, the embodiment of the invention provides pesticide granules for preventing and killing duckweed in lotus root fields, and the granules comprise the following components in percentage by weight: 2-6% of prometryn, 0.75-2.25% of clomazone, 0.1-0.3% of penoxsulam, 1-3% of a composite emulsifying agent, 2-5% of a composite film forming agent, 1-3% of a solvent and the balance of a composite carrier, wherein the composite emulsifying agent is as follows: mixtures of calcium dodecylbenzenesulfonate (Nanjing chemical Co., ltd.), castor oil polyoxyethylene ether Emulson CO25 (Nannong chemical Co., ltd.), CEREWIN T50V (tridecyl alcohol polyoxyethylene ether, nanford Co., ltd.), TERMUL 5500 (EO/PO block polyether, thailand IVL Co.); the composite film forming agent comprises: polyvinyl alcohol PVA100-84 (China petrochemical great wall energy chemical industry Co., ltd.), microcrystalline cellulose-sodium carboxymethyl cellulose composite Avicel CL-611 (America Co., ltd.), pure acrylic ester polymer emulsion 851 (Guangzhou Fangji Fine chemical industry Co., ltd.); the composite carrier is as follows: 20-30% of hollow glass beads (3M company in the United states), 10-15% of potassium chloride, 300-800% of sodium carboxymethylcellulose, 5-10% of calcium lignosulfonate Borderperse ca-sa (Norway Boleikudzuvine company), 3-10% of No. 58 paraffin powder and the balance of attapulgite. The inventor finds that the prometryn, clomazone and penoxsulam are taken as active ingredients to prepare granules through a large number of researches, and under the dosage proportion, lotus roots Tian Fuping with the water depth of 0.1-2 meters can be well prevented and removed, and the duckweed prevention and control problem when the lotus roots Tian Shuishen are 0.5-2 meters is well solved. In some preferred embodiments prometryn: clomazone: penoxsulam = 4:1.5:0.2, the content of which accounts for 2.85-8.55% of the total content of the granule.
Further, the composite emulsifier is calcium dodecyl benzene sulfonate: emulson CO25: CEREWIN T50V: terminal 5500=8: 2:3:2, the content of which is 1-3% of the total content of the granule.
Further, the composite film forming agent polyvinyl alcohol PVA100-84: microcrystalline cellulose-sodium carboxymethyl cellulose complex Avicel CL-611: pure acrylate polymer emulsion 851=1: 1:5, the content of the extract accounts for 2-5% of the total content of the granule.
Further, the composite carrier comprises 30% of hollow glass beads, 10% of potassium chloride, 300-8003% of sodium carboxymethylcellulose, 5% of calcium lignosulfonate Borderperse ca-sa, 5% of No. 58 paraffin powder and the balance of attapulgite.
Further, the preferable scheme of the granule is as follows: 4% of prometryn, 1.5% of clomazone, 0.2% of penoxsulam, 2% of a composite emulsifier, 4% of a composite film forming agent, 3% of No. 15 white oil and the balance of a composite carrier.
Further, the composite carrier processing method comprises the following steps: 30 percent of hollow glass beads, 10 percent of potassium chloride, 300 to 800 percent of sodium carboxymethyl cellulose, 5 percent of calcium lignosulfonate Borderperse ca-sa, 5 percent of No. 58 paraffin powder and the balance of attapulgite are uniformly mixed in a mixing kettle, and the mixture is prepared into 2 to 3 millimeter particles through a pan-type granulator, thus obtaining the composite carrier.
Further, the hollow glass microsphere has a diameter of 20-40 microns.
In another aspect, the invention provides a method for preparing the granule, which specifically comprises the following steps:
s1: preparation of composite carrier: uniformly mixing 20-30% of hollow glass beads, 10-15% of potassium chloride, 3-5% of sodium carboxymethylcellulose, 5-10% of calcium lignosulfonate Bordersperse ca-sa, 3-10% of No. 58 paraffin powder and the balance of attapulgite according to a proportion, and preparing into 2-3 mm particles by a pan granulator to obtain a composite carrier A;
s2: uniformly mixing prometryn, clomazone, penoxsulam, a compound emulsifier and a solvent, and grinding by a nano sand mill until D90=500 nanometers to obtain an active ingredient dispersion liquid B;
s3: adding the composite carrier A prepared in the step S1 into a pan-type granulator, adding the active ingredient dispersion liquid B prepared in the step S2 into the pan-type granulator under the condition that the pan-type granulator rotates, continuing to rotate the pan-type granulator until the active ingredient dispersion liquid B is completely adsorbed by the composite carrier A, adding a composite film forming agent, and continuing to rotate the pan-type granulator until the composite film forming agent is completely formed, thereby obtaining the granule.
Further, the granules are used for preventing and removing lotus roots Tian Fuping.
The embodiment of the invention has the following advantages:
the pesticide granule provided by the invention can float on the surface of water, wherein the pesticide active ingredient can be slowly released on the water surface, and has a very good effect on preventing and killing duckweed in lotus root fields.
The pesticide granule provided by the invention can have a very good control effect on duckweed in lotus root fields with the water depth of 0.1-2 meters, and is highly safe for lotus roots.
Detailed Description
Other advantages and advantages of the present invention will become apparent to those skilled in the art from the following detailed description, which, by way of illustration, is to be read in connection with certain specific embodiments, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. In the following examples and comparative examples, all percentages are by weight unless otherwise indicated.
Example 1
4% of prometryn, 1.5% of clomazone, 0.2% of penoxsulam, 2% of a composite emulsifier, 4% of a composite film forming agent, 3% of No. 15 white oil and the balance of a composite carrier.
Wherein the composite emulsifier is: calcium dodecylbenzenesulfonate: castor oil polyoxyethylene ether Emulson CO25: CEREWIN T50V: TERMUL 5500=8: 2:3:2; the composite film forming agent comprises: polyvinyl alcohol PVA100-84: microcrystalline cellulose-sodium carboxymethyl cellulose complex Avicel CL-611: pure acrylate polymer emulsion 851=1: 1: 5; the composite carrier is as follows: 30% of hollow glass beads, 10% of potassium chloride, 300-800% of sodium carboxymethylcellulose, 5% of calcium lignosulfonate Bordersperse ca-sa, 5% of No. 58 paraffin powder and the balance of attapulgite are uniformly mixed according to a proportion, and are prepared into 2-3 mm particles through a pan granulator to obtain a composite carrier; the prometryn, clomazone, penoxsulam, composite emulsifier and solvent are uniformly mixed, and are ground by a nano sand mill until D90=500 nanometers, so as to obtain an active ingredient dispersion liquid; adding the composite carrier into a pan-type granulator, adding the active ingredient dispersion liquid into the pan-type granulator under the condition that the pan-type granulator rotates, continuing to rotate the pan-type granulator until the active ingredient dispersion liquid is completely adsorbed by the composite carrier, adding the composite film forming agent, and continuing to rotate the pan-type granulator until the composite film forming agent is completely formed into films, thereby obtaining the granule.
Example 2
2% of prometryn, 0.75% of clomazone, 0.1% of penoxsulam, 1% of a composite emulsifier, 2% of a composite film forming agent, 1% of No. 15 white oil and the balance of a composite carrier.
Wherein the composite emulsifier, the composite film forming agent and the preparation method are exactly the same as those of the embodiment 1; the composite carrier is as follows: 20% of hollow glass microsphere, 15% of potassium chloride, 300-800% of sodium carboxymethylcellulose, 10% of calcium lignosulfonate Borderperse ca-sa, 10% of No. 58 paraffin powder and the balance of attapulgite, and the preparation method is the same as that of example 1.
Example 3
6% of prometryn, 2.25% of clomazone, 0.3% of penoxsulam, 3% of a composite emulsifier, 5% of a composite film forming agent, 3% of No. 15 white oil and the balance of a composite carrier.
Wherein the composite emulsifier, the composite film forming agent and the preparation method are exactly the same as those of the embodiment 1; the composite carrier is as follows: 15% of hollow glass microsphere, 7.5% of potassium chloride, 300-800.5% of sodium carboxymethylcellulose, 7.5% of calcium lignosulfonate Bordersperse ca-sa, 3% of No. 58 paraffin powder and the balance of attapulgite, and the preparation method is the same as that of example 1.
Comparative example 1
This comparative example was prepared as in example 1, except that prometryn, clomazone, penoxsulam, composite emulsifier, and solvent were mixed uniformly, and ground by a nano sand mill until d90=15 μm, otherwise exactly the same as in example 1.
Comparative example 2
This comparative example was prepared as in example 1, except that prometryn, clomazone, penoxsulam, composite emulsifier, and solvent were mixed uniformly, and ground by a nano sand mill until d90=5 μm, otherwise exactly the same as in example 1.
Comparative example 3
4% of prometryn, 0.2% of penoxsulam, 1.5% of clomazone, 5% of sodium lignin sulfonate, 3% of sodium dodecyl sulfate, 3% of white carbon black and the balance of attapulgite are uniformly mixed, crushed by air flow, then kneaded by adding water, granulated and dried to prepare granules.
Comparative example 4
4% of prometryn, 0.2% of penoxsulam, 1.5% of clomazone, 15% of sodium lignin sulfonate, 3% of sodium dodecyl sulfate, 3% of polycarboxylate dispersant Atlox metaperse 550S, 3% of white carbon black and the balance of attapulgite, and after uniform mixing, carrying out jet milling, then adding water for kneading, granulating and drying to prepare the water dispersible granule.
Comparative example 5
4% of prometryn, 0.2% of penoxsulam, 1.5% of clomazone, 5% of tristyrylphenol polyoxyethylene ether (EO=16) phosphate triethanolamine salt, 2% of isomeric tridecanol polyoxyethylene ether (EO=6), 5% of ethylene glycol, 0.2% of organosilicon defoamer, 0.15% of xanthan gum, 0.2% of sodium benzoate and the balance of water, and preparing a suspending agent after sanding.
Comparative example 6
The procedure of example 1 was repeated except that the complex emulsifier of example 1 was changed to NP-10.2%.
Comparative example 7
The procedure of example 1 was repeated except that the composite film-forming agent of example 1 was changed to polyvinyl alcohol 1788 4%.
Comparative example 8
The procedure is exactly as in example 1, except that the composite carrier of example 1 is replaced with expanded perlite.
2 test case
2.1 evaluation of the Combined action
The test adopts a Colby method to test the activity of three herbicides after mixed use, and the mixed calculation is shown as E0 (%) =X X Y Z/100 (n-1), wherein X represents the actual weed survival rate of penoxsulam; y represents the measured weed survival rate of clomazone; z represents the measured weed survival rate of prometryn; n represents the amount of the compound herbicide; e0 represents the survival rate of the mixed theory; e represents the observed survival rate.
When E-E0< -10%, the synergistic effect is shown; E-E0>10% indicates antagonism; E-E0 is between + -10%, which indicates additive effect of drug production after compounding.
TABLE 1 indoor Activity of penoxsulam, clomazone and prometryn for control of Duckweed
As can be seen from Table 1, the prevention effect of penoxsulam, clomazone and prometryn on duckweed under the corresponding single active substance dosage is 29-42%,31-51%,56-72% through indoor bioassay, and good field application value is not achieved. By compounding the three herbicides according to the proportion of different dosages, it is found that in some compound combinations (penoxsulam+clomazone+prometryn=15+112.5+300, 15+112.5+450, 15+225+300, 15+225+450, 30+112.5+300, 30+225+450, 30+225+600, 45+225+300), obvious synergism occurs, and the synergism is more obvious at lower dosages.
2.1 control index and detection result
With reference to HG/T2467.12-2003 "standard writing Specification for pesticide granule products", corresponding indexes required in the standard are detected according to a detection method specified in the standard, and the detection indexes and results of the pesticide granule prepared in example 1 of the present invention are shown in Table 1.
TABLE 2 control index and test results of granules
As can be seen from table 2, each detection result meets the standard requirement of the granule.
2.2 stability Performance test
Weighing 50 g of the sample of the example 1, adding the sample into a high-barrier bottle, sealing, placing the bottle in a constant temperature incubator at 54 ℃, detecting mass fractions of three pesticide active ingredients by using a high performance liquid chromatograph after 14 days, and calculating the heat storage decomposition rate.
TABLE 3 detection results of active ingredient before and after heat storage
TABLE 4 decomposition rate by heat storage
The result shows that the decomposition rate of the three effective components of clomazone, penoxsulam and prometryn after heat storage of the granule prepared by the embodiment 1 of the invention is less than 5%, and the granule meets the quality requirement of pesticide granules.
2.3 Release Rate test
In order to effectively test the release condition of the active ingredients in the pesticide granules obtained by the invention in water, the content of the active ingredients in the granules applied to the water is detected respectively for 15 days, 30 days and 60 days. And calculating the total release rate of the active ingredients in the corresponding time node granules:
total release rate = (w0×m0-wn× mn)/w0×m0
w0 is the total mass fraction of the initial active ingredients;
m0 is the initial particle weight;
wn, total mass fraction of active ingredients at corresponding time (n=15 days, 30 days, 60 days);
mn: the weight of the particles at the corresponding time (n=15 days, 30 days, 60 days).
The specific operation method comprises the following steps: and (3) weighing a certain weight of sample in a plastic water tank with the length and width of 100 cm and the height of 120 cm at the scale of 100 cm, scattering the sample on the surface of water, respectively standing for 15 days, 30 days and 60 days, fishing out the granules by using a screen, putting the granules into a weighing bottle, drying the granules until the water content of the granules is less than 2.0% at 54 ℃, and detecting the content of three effective components in the pesticide granules by using a high performance liquid chromatograph.
TABLE 5 active ingredient content and Total Release Rate
As can be seen from Table 5, the granules prepared in example 1 of the present invention showed total release rates of the active ingredients of 29.8%, 48.7% and 61.5% after 15 days, 30 days and 60 days of administration into water; after the granules prepared in the example 2 are applied to water for 15 days, 30 days and 60 days, the total release rate of the active ingredients in the granules is 22.7%, 42.3% and 52.2% respectively; after the granules prepared in the example 3 are applied to water for 15 days, 30 days and 60 days, the total release rate of the active ingredients in the granules is 20.7%, 34.8% and 50.2% respectively; after the granules prepared in the comparative example 6 are applied to water for 15 days, 30 days and 60 days, the total release rate of the active ingredients in the granules is 26.4%, 45.5% and 55% respectively; the granule prepared in comparative example 7 was immediately dispersed in water without floating and sustained release; the granule prepared in comparative example 8 can float on the water surface, but the active ingredient in the granule is released 90.8% after 15 days and 97.4% after 30 days, and has no slow release effect.
2.4 emulsifier wettability test
Mixing the emulsifier calcium dodecyl benzene sulfonate, emulson CO25 and CEREWIN T50V, TERMUL 5500 according to different proportions to obtain a composite emulsifier, diluting the composite emulsifier with tap water 1000 times to obtain an emulsifier diluent, taking the emulsifier diluent by a1 ml dropper, respectively dripping one drop of the emulsifier diluent onto leaf surfaces of lotus leaves and duckweed, and observing the wetting condition.
TABLE 6 wettability of different emulsifier ratios to lotus leaf and duckweed
Nail (A): calcium dodecyl benzene sulfonate, b: emulson CO25, C: CEREWIN T50V: butyl: TERMUL 5500
Experiments show that after four surfactants of calcium dodecyl benzene sulfonate, emulson CO25 and CEREWIN T50V, TERMUL 5500 are mixed according to a certain proportion, the water solution of the surfactants can well wet the duckweed leaves, but not wet the lotus roots, and the selected surfactants can wet the duckweed leaves and also wet the lotus roots.
3. Field efficacy and safety test
3.1 field test 1
Test agent: granules of examples 1-3, comparative examples 1-8, 50% prometryn suspension, 5% penoxsulam dispersible oil suspension, 46% clomazone emulsifiable concentrate.
Test date: 2022, 6 and 7 days
Test site: hubei xiantao city
Control object: duckweed
The test method comprises the following steps: the field duckweed is selected to generate a more uniform lotus root field, and other herbicides are not used in the test in the season. The water depth was 20 cm and three replicates were set for each treatment of 100 square meters. The application method comprises uniformly sprinkling the granule on water surface, observing death condition of herba Spirodelae 15 days, 30 days and 60 days after administration, comparing safety of each preparation on rhizoma Nelumbinis and control effect on herba Spirodelae by fresh weight method, and the results are shown in Table 5.
TABLE 7 safety and efficacy results
Remarks: m is 50% prometryn suspending agent; 5% penoxsulam dispersible oil suspension; 46% clomazone emulsifiable concentrate.
From comparison of comparative examples 1-2 and examples 1-3, it was found that the control effect of comparative examples 1-2 on duckweed was much smaller than that of examples 1-3. The invention relates to a pesticide composition, which is characterized in that the particle size of the dispersing particle of the effective component of the pesticide has great influence on the control effect, the particle size of the effective component of the conventional pesticide formulation water dispersible granule and wettable powder in the industry is usually 15 microns, the particle size of the suspending agent and the particle size of the dispersible oil suspending agent are usually 5 microns, the particle size of the effective component is dispersed to D90 of less than 500 nanometers through a nano sand mill, and the control effect of the pesticide on duckweed can be obviously improved under the condition of the same dosage of the pesticide.
As can be seen from comparative examples 3 to 5, the control effect of the medicaments prepared in comparative examples 3 to 5 on duckweed is greater than 98% 15 days after administration, which is equivalent to that of example 1. However, the prevention effect on duckweed after 30 days of administration is as follows: 90.2%, 88.7% and 89.6%, and the prevention effect on duckweed after 60 days of administration is respectively as follows: 78.2%, 77.4% and 74.1% which are obviously smaller than the control effect of the duckweed on the corresponding days of the examples 1-3. This is because the solubility of prometryn and penoxsulam in water is low, and they are dispersed in water in the form of solid particles, which sink to the soil surface of the water bottom due to gravity, while duckweed grows on the surface of the water, so that there is insufficient pesticide active ingredient in contact with duckweed, and when the concentration of pesticide active ingredient in the water layer contacted by duckweed is less than the lethal concentration for duckweed, new duckweed will continue to grow and reproduce. The pesticide granule provided by the embodiment can always float on the surface of water, and the effective components in the pesticide granule can be slowly released on the water surface, so that the pesticide granule contacts with duckweed, and can continuously kill duckweed growing on the water surface.
TABLE 8 control Effect of different aqueous layers on duckweed
Remarks: m is 50% prometryn suspending agent; 5% penoxsulam dispersible oil suspension; 46% clomazone emulsifiable concentrate.
As can be seen from Table 8, when the water depth is 20 cm, the examples 1-3 are not obviously different from the comparative examples 1-8, and the prevention effect on duckweed is more than 95%; when the water depth is 50 cm, the control effect of the duckweed in the embodiment 1-3 still reaches 99.5%, and the control effect of the duckweed in the comparative example is reduced to a certain extent; when the depth of the water is 100 cm, the control effect of the duckweed in the examples 1-3 is obviously better than that of the duckweed in the comparative examples 1-8.
3.2 field trial 2
Test agent: granules of examples 1-3, comparative examples 1-8, 50% prometryn suspension, 5% penoxsulam dispersible oil suspension, 46% clomazone emulsifiable concentrate.
Test date: 2022, 7 and 12 days
Test site: jiangsu Baozi county
Control object: duckweed
The test method comprises the following steps: test method is the same as 3.1
TABLE 9 safety and efficacy results
Remarks: m is 50% prometryn suspending agent; 5% penoxsulam dispersible oil suspension; 46% clomazone emulsifiable concentrate.
As can be seen from the test data in Table 9, the control effect of example 1 on duckweed reaches a high level at 15 days, 30 days and 60 days after administration, and is very safe to lotus roots.
The control effect of comparative examples 1-2 on duckweed at 15 days, 30 days and 60 days after administration is significantly inferior to that of example 1 at the corresponding time, but the control effect of comparative examples 1-2 on duckweed is not significantly reduced with the lapse of time, because the pesticide active ingredient in the granules prepared by the present processing technique can be slowly released on the water surface.
The control effect of comparative examples 3-5 on duckweed reached a higher level 15 days after administration, and the control effects were 97.4%, 96.2% and 95.3% respectively, but the control effect on duckweed was remarkably reduced after administration for 30 days and 60 days with the prolonged period of time.
While the invention has been described in detail in the foregoing general description and specific examples, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.

Claims (9)

1. The pesticide granule for preventing and killing duckweed in lotus root fields is characterized by comprising the following components in percentage by weight: 2-6% of prometryn, 0.75-2.25% of clomazone, 0.1-0.3% of penoxsulam, 1-3% of a composite emulsifying agent, 2-5% of a composite film forming agent, 1-3% of a solvent and the balance of a composite carrier, wherein the composite emulsifying agent is as follows: a mixture of calcium dodecylbenzenesulfonate, castor oil polyoxyethylene ether, CEREWIN T50V, TERMUL 5500; the composite film forming agent comprises: a mixture of polyvinyl alcohol PVA100-84, microcrystalline cellulose-sodium carboxymethylcellulose complex Avicel CL-611, pure acrylic acid ester polymer emulsion 851; the composite carrier is as follows: 20-30% of hollow glass beads, 10-15% of potassium chloride, 3-5% of sodium carboxymethylcellulose, 5-10% of calcium lignosulfonate Borderperse ca-sa, 3-10% of No. 58 paraffin powder and the balance of attapulgite.
2. The agricultural chemical granule for preventing and removing duckweed in lotus root fields as claimed in claim 1, wherein the prometryn: clomazone: penoxsulam = 4:1.5:0.2, the content of which accounts for 2.85-8.55% of the total content of the granule.
3. The agricultural chemical granule for preventing and killing duckweed in lotus root field as claimed in claim 1, wherein the composite emulsifier comprises calcium dodecylbenzenesulfonate: emulson CO25 CEREWIN T50V terminal 5500=8: 2:3:2, the content of which is 1-3% of the total content of the granule.
4. The pesticide granule for preventing and killing duckweed in lotus root fields according to claim 1, wherein the polyvinyl alcohol PVA100-84 in the composite film forming agent is as follows: microcrystalline cellulose-sodium carboxymethyl cellulose complex Avicel CL-611: pure acrylate polymer emulsion 851=1: 1:5, the content of the extract accounts for 2-5% of the total content of the granule.
5. The agricultural chemical granule for preventing and killing duckweed in lotus root fields as claimed in claim 1, wherein the granule comprises, in weight percent: 4% of prometryn, 1.5% of clomazone, 0.2% of penoxsulam, 2% of a composite emulsifier, 4% of a composite film forming agent, 3% of No. 15 white oil and the balance of a composite carrier.
6. The pesticidal granule for controlling duckweed in lotus root fields according to claim 1 or 5, wherein the composite carrier comprises, in weight percent: 30% of hollow glass beads, 10% of potassium chloride, 300-8003% of sodium carboxymethylcellulose, 5% of calcium lignosulfonate Borderperse ca-sa, 5% of No. 58 paraffin powder and the balance of attapulgite.
7. The pesticidal granule for controlling duckweed in lotus root fields according to claim 1 or 5, wherein the composite carrier processing method is as follows: 30 percent of hollow glass beads, 10 percent of potassium chloride, 3 percent of sodium carboxymethylcellulose, 5 percent of calcium lignosulfonate Bordersperse ca-sa, 5 percent of No. 58 paraffin powder and the balance of attapulgite are uniformly mixed in a mixing kettle, and the mixture is prepared into 2-3 mm particles through a pan granulator, thus obtaining the composite carrier.
8. The agricultural chemical granule for preventing and killing duckweed in lotus root field as claimed in claim 1, wherein the hollow glass micro-beads have a diameter of 20-40 μm.
9. The preparation method of the granule is characterized by comprising the following steps:
s1: preparation of composite carrier: uniformly mixing 20-30% of hollow glass beads, 10-15% of potassium chloride, 3-5% of sodium carboxymethylcellulose, 5-10% of calcium lignosulfonate Bordersperse ca-sa, 3-10% of No. 58 paraffin powder and the balance of attapulgite according to a proportion, and preparing into 2-3 mm particles by a pan granulator to obtain a composite carrier A;
s2: uniformly mixing prometryn, clomazone, penoxsulam, a compound emulsifier and a solvent, and grinding by a nano sand mill until D90=500 nanometers to obtain an active ingredient dispersion liquid B;
s3: adding the composite carrier A prepared in the step S1 into a pan-type granulator, adding the active ingredient dispersion liquid B prepared in the step S2 into the pan-type granulator under the condition that the pan-type granulator rotates, continuing to rotate the pan-type granulator until the active ingredient dispersion liquid B is completely adsorbed by the composite carrier A, adding a composite film forming agent, and continuing to rotate the pan-type granulator until the composite film forming agent is completely formed into films, thereby obtaining the granules;
the granule is the pesticide granule for preventing and killing duckweed in lotus root fields according to any one of claims 1 to 5.
CN202311555128.XA 2023-11-21 2023-11-21 Pesticide granule for preventing and killing duckweed in lotus root field and preparation method thereof Pending CN117814247A (en)

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