CN110771613A - Weeding composition containing clopyralid and terbuthylazine and application thereof - Google Patents

Weeding composition containing clopyralid and terbuthylazine and application thereof Download PDF

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Publication number
CN110771613A
CN110771613A CN201911218103.4A CN201911218103A CN110771613A CN 110771613 A CN110771613 A CN 110771613A CN 201911218103 A CN201911218103 A CN 201911218103A CN 110771613 A CN110771613 A CN 110771613A
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Prior art keywords
terbuthylazine
clopyralid
millet
composition containing
herbicidal composition
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CN201911218103.4A
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CN110771613B (en
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王根平
李秉华
程汝宏
张婷
刘国庆
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Grain Research Institute of Hebei Academy of Agriculture and Forestry Sciences
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Grain Research Institute of Hebei Academy of Agriculture and Forestry Sciences
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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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings

Abstract

The weeding composition containing clopyralid and terbuthylazine and the application thereof are characterized in that the composition consists of 10-90% of active ingredients, the balance of auxiliary agents and carriers according to weight percentage, wherein the active ingredients comprise (1-2): (1-60) clopyralid and terbuthylazine. The field test result of the composition shows that the total control effect on the fresh weight of the weeds in the field reaches more than 95% under the dosage of 500 g/hectare of clopyralid terbuthylazine for stem and leaf application of millet and broom corn millet at the 2-5 leaf stage and the 2-4 leaf stage of the weeds, the millet and the broom corn millet grow normally without the symptom of phytotoxicity, and the composition can be safely used for the post-seedling treatment of the millet field and the broom corn millet field and has obvious weeding yield-increasing effect and labor-saving and time-saving effects.

Description

Weeding composition containing clopyralid and terbuthylazine and application thereof
Technical Field
The invention belongs to the technical field of pesticides, and relates to a weeding composition, in particular to a weeding composition containing clopyralid and terbuthylazine and application thereof, which is used for preventing and killing off field weeds in post-seedling stem and leaf treatment of millet fields and broom corn fields.
Background
At present, 2, 4-D butyl ester, dimethyl tetrachlorosodium and the like are widely used as herbicides for post-emergence weeding in millet fields, but the herbicides are only effective on partial broad-leaved weeds, and have the problems of low safety on millet in the using process (Yangzhou, Ningyuei, Guorufeng, etai.2, 4-D butyl ester has influence on the growth form indexes of the millet [ J ]. Chinese agriculture report, 2015,31(30):132 and 138.), sensitive plant phytotoxicity caused by easy drift, difficult cleaning of spraying instruments and the like. The broom corn millet field is lack of safe post-emergence stem and leaf treatment herbicides.
Clopyralid is the english generic name for clopyralid, chemical name: 3, 6-dichloropyridine-2-carboxylic acid belongs to heterocyclic herbicides, and sensitive weeds can wither and die after being absorbed, and finally die. Clopyralid has a good effect of controlling dicotyledonous weeds such as endive, vetch, sticktight and the like in the family of Compositae and Leguminosae (Guojian. clopyralid has an effect of controlling spiny weeds and endive in spring rape fields. weed science, 2009, 1). Clopyralid and other herbicides are compounded to form some herbicidal compositions, for example, CN106719671A reports a pesticide composition containing clopyralid and fluoroglycofen-ethyl and application thereof, and the composition is used for controlling broadleaf weeds in rape fields; ZL201310473414.1 reports that a topramezone-clopyralid compounded corn field herbicide has obvious synergistic effect on field weeds after two effective components are compounded according to a certain proportion.
Terbuthylazine, the common english name for terbuthylazine, chemical name: 2-chloro-4-tert-butylamino-6-ethylamino-1, 3, 5-triazine, belongs to triazine compounds, and is used for preventing and killing various weeds. The action mechanism is that through PS II, D1 protein is used as an action target to inhibit the photosynthesis of plants. Terbuthylazine is absorbed mainly by plant root, and can be treated by soil before sowing, or applied to stem and leaf after seedling. Terbuthylazine is mainly used for weeding in corn fields, for example, CN101142914 reports a nicosulfuron terbuthylazine compound corn field herbicide; CN106665611A discloses a post-emergence herbicidal composition containing 2-methyl-4-chloroisooctyl ester, florasulam and terbuthylazine; CN105379733B discloses a flufenacet-terbuthylazine compound cornfield herbicide.
Millet and broom corn millet are sensitive to most herbicides, affecting the yield and quality of crops. At present, the report of the herbicide composition compounded by terbuthylazine and clopyralid does not exist, and the technology of compounding terbuthylazine and clopyralid and using the terbuthylazine and clopyralid in millet fields and broom corn fields is lacked.
Disclosure of Invention
The invention aims to provide an efficient, low-toxicity and safe post-emergence stem and leaf treatment herbicide for millet fields and broom corn fields, which can improve the yield and quality of crops.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a weeding composition containing clopyralid and terbuthylazine comprises, by weight, 10-90% of active ingredients, the balance of auxiliaries and carriers, wherein the active ingredients comprise, by weight, (1-2): (1-60) clopyralid and terbuthylazine.
Preferably, the weight ratio of the clopyralid to the terbuthylazine is (1-2): (2-24).
More preferably, the weight ratio of the clopyralid to the terbuthylazine is 1: 8.
the auxiliary agent is one or any combination of a safener, a wetting agent, a dispersing agent, an adhesive, an emulsifying agent, a penetrating agent and the like.
The safener is selected from one or any combination of CGA-28725, CGA-145138, cloransulam, isoxadifen, cyclopropanesulfonamide, R-25788, MG-191, cloquintocet, gibberellin, 1, 8-naphthalic anhydride, brassinolide, CGA-154281, Hoe-70542, clethodim, 2-chloro-4-trifluoromethyl-1, 3-thiazole-5-benzyl carboxylate, dichloroacetyl diisopropylamine, 3-dichloroacetyl-5- (2-furyl) -2, 2-dimethyl-1, 3-oxazolidine, mefenpyr and antidote T.
The composition is one of suspending agent, dry suspending agent, wettable powder, water dispersible granule and suspoemulsion.
In a crop field, the weeding composition is used for carrying out stem and leaf treatment after seedling, and is applied to crops (millet and broom corn millet) at the 2-5 leaf stage and weeds at the 2-4 leaf stage, so that the weeding effect on weeds can be obviously improved, the phytotoxicity of herbicides is avoided, and safe weeding is realized.
The crop field comprises a millet field and a broom corn field.
The invention has the beneficial effects that:
the combined action of the clopyralid and the terbuthylazine after being mixed is evaluated by a Gowing method, and the result shows that the combined action of the clopyralid and the terbuthylazine after being mixed according to the proportion of (1-2) to (1-60) is more than 0 for weed control effect, belonging to the addition or synergy effect.
The field test result of the composition shows that the total control effect on the fresh weight of the weeds in the field reaches over 95 percent under the dosage of 500 g/hectare of clopyralid terbuthylazine by using stem and leaf medicines in the 2-5 leaf period of millet and broom corn millet and the 2-4 leaf period of the weeds. The millet and the broom corn millet grow normally, have no phytotoxicity symptom, can be safely used for post-treatment of millet fields and broom corn millet fields, and have obvious weeding and yield increasing effects and labor and time saving effects.
The weeding composition provided by the invention has the advantages of improved weed control effect, obvious synergistic effect and wide weed control spectrum: after the herbicidal composition clopyralid and terbuthylazine are combined according to a certain proportion, the herbicidal composition unexpectedly shows an obvious combined synergistic effect on common annual weeds in millet fields and broom corn fields, can obviously improve the control effects on common weeds in millet fields and broom corn fields, such as crab grass, green bristlegrass, redroot amaranth, Japanese thistle and the like, the control effect on the redroot amaranth is improved by 14.1 percent to the maximum extent, the control effect on the Japanese thistle is improved by 12.1 percent to the maximum extent, the control effect on gramineous weeds is improved by an unexpected additive effect, and the control effect is improved by 13.7 percent to the maximum extent. The weeding composition can prevent and kill various gramineous weeds and broad-leaved weeds in the field, and avoids the problem that the control effect of one agent is not ideal for some weeds (see tables 2, 3, 4 and 5).
The weeding composition disclosed by the invention is high in safety on crops, and avoids drifting phytotoxicity on millet, broom corn millet and sensitive crops around: compared with the common herbicide, the yield of the millet and the broom corn millet is respectively increased by 26.4-67.1kg and 35.6-82.8 kg; compared with the clear water, the maximum yield increase rates of millet and broom corn millet respectively reach 103.1% and 97.7% (see tables 6 and 7), and the social benefit and the economic benefit are obvious. The crop has no phytotoxicity symptom after the composition is applied in the test process; nearby other crops, such as corn, soybean, peanut, cotton and the like, do not have the symptom of drift phytotoxicity; the two medicaments do not cause phytotoxicity to millet, broom corn millet, afterreap crops or peripheral sensitive crops under the recommended dosage.
The herbicidal composition of the present invention increases the yield and quality of crops: the product and the application technology provided by the invention can effectively prevent and control weeds in the millet field and the broom corn field, effectively avoid the influence of the herbicide on the yield and the quality of crops, remarkably improve and enhance the nutritive value of the crops and harvest unexpected preferences (see tables 6 and 7).
Detailed Description
The present invention will be further described with reference to the following examples. The examples given are intended to further illustrate the combinations and implementations of the invention, and do not set any limit to the scope of the invention.
In the following examples, percentages are by weight, unless otherwise indicated; the carrier of the invention is a carrier which is helpful for applying active ingredients, such as water, kaolin, attapulgite, argil, white clay, light calcium carbonate, corn starch, white carbon black and the like.
Detailed description of the preferred embodiments
EXAMPLE 160% Triton Dichloropicolinic acid suspension (1: 8)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 6.67% of clopyralid, 53.33% of terbuthylazine, 0.02% of brassinolide, 2.5% of alkylphenol polyoxyethylene phosphate, 1% of Morwet EFW, 1% of xanthan gum, 200006% of polyethylene glycol, BX 8221% and water in balance.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and water according to a weight ratio, crushing by a ball mill and a sand mill, detecting that the particle diameter of the material reaches 2 microns, processing by a high-shear emulsifying kettle and a homogenizing mixer, and preparing the 60% clopyralid-terbuthylazine suspending agent after the detection is qualified.
EXAMPLE 250% Dichloropicolinic acid terbuthylazine dry suspension (1: 4)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 10% of clopyralid, 40% of terbuthylazine, 4.5% of isoxadifen, PEG 80008%, 25% of Ufoxane, 70G 4% of YUS-EP, and the balance of kaolin.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the weight proportion, crushing by a sand mill, removing dust from tail gas by a spray granulator and a dryer, emptying, and preparing into the 50 percent dry suspending agent of clopyralid terbuthylazine after passing the detection.
EXAMPLE 380% Tripyric acid terbuthylazine wettable powder (1: 3)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 20% of clopyralid, 60% of terbuthylazine, DT-8826%, 1.5% of Petro AA, 5% of white carbon black and the balance of kaolin.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the weight ratio, fully mixing and crushing by a jet mill, and preparing 80% clopyralid terbuthylazine wettable powder after passing detection.
Example 490% Triton (TM) Dichloropicolinic acid Water dispersible granules (2: 58)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 3% of clopyralid, 87% of terbuthylazine, SOPA S-2702%, JFC 3%, 3% of polyvinyl alcohol and the balance of argil.
The process comprises the following steps: taking the terbuthylazine raw drug and the clopyralid raw drug according to the formula, drying, weighing and crushing the terbuthylazine raw drug and the clopyralid raw drug, sequentially putting the terbuthylazine raw drug, the auxiliary agent and the filler into a preparation kettle in proportion, crushing and uniformly mixing the terbuthylazine raw drug, the auxiliary agent and the filler by a high-speed shearing machine, adding the binder and the water, uniformly mixing the mixture, granulating, drying and screening the mixture, and obtaining a finished product after quality inspection.
EXAMPLE 540% Triton Dichloropicolinic acid suspension (1: 1)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 20% of clopyralid, 20% of terbuthylazine, 1.5% of Diwatex XP, 5.5% of white carbon black, 15% of sodium lignosulfonate and the balance of water.
The process comprises the following steps: mixing the original medicine, the auxiliary agent, the filler and the water according to a weight ratio, crushing by a ball mill and a sand mill, detecting that the particle diameter of the material reaches 2 microns, processing by a high-shear emulsifying kettle and a homogenizing mixer, and preparing the 40% clopyralid-terbuthylazine suspending agent after the detection is qualified.
EXAMPLE 650% Dichloropicolinic acid terbuthylazine dry suspension (1: 60)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 0.82% of clopyralid, 49.18% of terbuthylazine, 1% of xanthan gum, 6% of white carbon black, 4% of ethylene glycol and the balance of white clay.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the weight proportion, crushing by a sand mill, removing dust from tail gas by a spray granulator and a dryer, emptying, and preparing into the 50 percent dry suspending agent of clopyralid terbuthylazine after passing the detection.
EXAMPLE 790% Tripyric acid terbuthylazine wettable powder (1: 60)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 1.48 percent of clopyralid, 88.52 percent of terbuthylazine, 122 percent of K, Morwet D-5004 percent of light calcium and the balance of light calcium.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the weight ratio, fully mixing and crushing by a jet mill, and preparing 90% clopyralid terbuthylazine wettable powder after passing detection.
Example 888% Dichloropicolinic acid terbuthylazine Water dispersible granules (1: 5)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 14.67% of clopyralid, 73.33% of terbuthylazine, 10026% of D, 20015% of W and the balance of corn starch.
The process comprises the following steps: taking the terbuthylazine raw drug and the clopyralid raw drug according to the formula, drying, weighing and crushing the terbuthylazine raw drug and the clopyralid raw drug, sequentially putting the terbuthylazine raw drug, the auxiliary agent and the filler into a preparation kettle in proportion, crushing and uniformly mixing the terbuthylazine raw drug, the auxiliary agent and the filler by a high-speed shearing machine, adding the binder and the water, uniformly mixing the mixture, granulating, drying and screening the mixture, and obtaining a finished product after quality inspection.
Example 988% Triton Dichloropicolinic acid suspension (1: 4)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 17.6 percent of clopyralid, 70.4 percent of terbuthylazine, 1.5 percent of dibutyl naphthalene sodium sulfonate, 4 percent of sorbitol, 0.2 percent of sodium alginate, 1 percent of bentonite, F381.3 percent, and water for balancing.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and water according to a weight ratio, crushing by a ball mill and a sand mill, detecting that the particle diameter of the material reaches 2 microns, processing by a high-shear emulsifying kettle and a homogenizing mixer, and preparing the 88% clopyralid-terbuthylazine suspending agent after the detection is qualified.
EXAMPLE 1070% Dichloropicolinic acid terbuthylazine dry suspension (2: 10)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 11.67% of clopyralid, 58.33% of terbuthylazine, 3% of Petro-AGS, 10% of NNO, 0.5% of palmitic acid and the balance of white clay.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the weight ratio, crushing by a sand mill, performing dust removal on tail gas by a spray granulator and a dryer, emptying, and preparing the 70% clopyralid-terbuthylazine dry suspending agent after passing the detection.
EXAMPLE 1155% Trifluzine Dichloropicolinate wettable powder (1: 8)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 6.11 percent of clopyralid, 48.89 percent of terbuthylazine, DT-8017 percent of white carbon black and kaolin for balancing.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the weight ratio, fully mixing and crushing by a jet mill, and preparing 55% clopyralid terbuthylazine wettable powder after passing the detection.
Example 1270% Triton hydrochloride Water dispersible granules (1: 6)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 10% of clopyralid, 60% of terbuthylazine, SS-26164%, 34753% of HOES, 60001% of polyethylene glycol and the balance of white carbon black.
The process comprises the following steps: taking the terbuthylazine raw drug and the clopyralid raw drug according to the formula, drying, weighing and crushing the terbuthylazine raw drug and the clopyralid raw drug, sequentially putting the terbuthylazine raw drug, the auxiliary agent and the filler into a preparation kettle in proportion, crushing and uniformly mixing the terbuthylazine raw drug, the auxiliary agent and the filler by a high-speed shearing machine, adding the binder and the water, uniformly mixing the mixture, granulating, drying and screening the mixture, and obtaining a finished product after quality inspection.
EXAMPLE 1375% Tripyric acid terbuthylazine suspension (1: 50)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 1.47% of clopyralid, 73.53% of terbuthylazine, UH 7523%, 20005% of agricultural emulsion, 1.5% of glycerol and the balance of water.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and water according to a weight ratio, crushing by a ball mill and a sand mill, detecting that the particle diameter of the material reaches 2 microns, processing by a high-shear emulsifying kettle and a homogenizing mixer, and preparing the 75% clopyralid-terbuthylazine suspending agent after the detection is qualified.
Example 1466% Tripyric dichloride Tebutazine Dry suspension (1: 60)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: clopyralid 1.08%, terbuthylazine 64.92%, Ablusol 7%, Sokalan HP-5018%, kaolin to make up the rest.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the weight proportion, crushing by a sand mill, removing dust from tail gas by a spray granulator and a dryer, emptying, and preparing the 66 percent clopyralid terbuthylazine dry suspending agent after passing detection.
EXAMPLE 1510% Tripyric dichloride terbuthylazine wettable powder (1: 4)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 2% of clopyralid, 8% of terbuthylazine, D-1108%, 122.5% of K, 9.5% of white carbon black and the balance of kaolin.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the weight ratio, fully mixing and crushing by a jet mill, and preparing 10% clopyralid terbuthylazine wettable powder after passing detection.
Example 1620% Triton (TM) Dichloropicolinic acid Water dispersible granules (1: 4)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 4% of clopyralid, 16% of terbuthylazine, 10041.8% of TERWET, TERSPERSE 27005.2% of ammonium sulfate and the balance of white carbon black.
The process comprises the following steps: taking the terbuthylazine raw drug and the clopyralid raw drug according to the formula, drying, weighing and crushing the terbuthylazine raw drug and the clopyralid raw drug, sequentially putting the terbuthylazine raw drug, the auxiliary agent and the filler into a preparation kettle in proportion, crushing and uniformly mixing the terbuthylazine raw drug, the auxiliary agent and the filler by a high-speed shearing machine, adding the binder and the water, uniformly mixing the mixture, granulating, drying and screening the mixture, and obtaining a finished product after quality inspection.
Example 1748% Tributine Dichloropicolinate suspension (1: 1)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 24% of clopyralid, 24% of terbuthylazine, 154% of AEO, 6006% of agricultural milk, 1% of carboxymethyl cellulose, 0.5% of polyoxypropylene glycerol ether, 3% of glycerol and the balance of water.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and water according to a weight ratio, uniformly mixing by a stirring kettle, performing high-speed shearing homogenization in a sand mill circulating sand mill and a high-shearing emulsification kettle, and preparing the 48% clopyralid-terbuthylazine suspending emulsion after passing detection.
Example 1855% Tributine Dichloropyridinate suspoemulsion (1: 60)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 0.90% of clopyralid, 54.10% of terbuthylazine, 48966% of Tersperse, 335% of Ningru, 2% of modified bentonite, 1% of macromolecular polycarboxylate, 3% of urea and the balance of water.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and water according to a weight ratio, uniformly mixing by a stirring kettle, performing high-speed shearing homogenization in a sand mill circulating sand mill and a high-shearing emulsification kettle, and preparing the 55% clopyralid-terbuthylazine suspending emulsion after passing detection.
Example 1960% Tripyric acid terbuthylazine suspoemulsion (1: 4)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 12% of clopyralid, 48% of terbuthylazine, O-306%, WA-403%, 1.5% of ammonium polyacrylate, 2.5% of glycerol and the balance of water.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and water according to a weight ratio, uniformly mixing by a stirring kettle, performing high-speed shearing homogenization in a sand mill circulating sand mill and a high-shearing emulsification kettle, and preparing the 60% clopyralid-terbuthylazine suspending emulsion after passing detection.
Example 2070% Triton Dichloropicolinic acid suspension (1: 9)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 7% of clopyralid, 63% of terbuthylazine, 22106% of Tersperse, SFR-70913%, 1.5% of potassium alginate, 3.5% of ethylene glycol, T-201% of agricultural emulsion and the balance of water.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and water according to a weight ratio, uniformly mixing by a stirring kettle, performing high-speed shearing homogenization in a sand mill circulating sand mill and a high-shearing emulsification kettle, and preparing the 70% clopyralid-terbuthylazine suspending emulsion after passing detection.
Example 2110% Dichloropicolinic acid terbuthylazine suspension (1: 16)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 0.59% of clopyralid, 9.41% of terbuthylazine, 0.01% of brassinolide, 1.2% of NNO, 1.7% of BX, 1% of xanthan gum, 4% of ethylene glycol and the balance of water.
The process comprises the following steps: mixing the original medicine, the auxiliary agent, the filler and the water according to a weight ratio, crushing by a ball mill and a sand mill, detecting that the particle diameter of the material reaches 2 microns, processing by a high-shear emulsifying kettle and a homogenizing mixer, and preparing the 10% clopyralid-terbuthylazine suspending agent after the detection is qualified.
EXAMPLE 2215% Dry suspension of Dichloropicolinic acid terbuthylazine (1: 4)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 3% of clopyralid, 12% of terbuthylazine, 10042.5% of TERWET, 4% of sodium lignosulfonate, 3% of ammonium sulfate, 4% of ethylene glycol and the balance of convex-concave soil.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the weight proportion, crushing by a sand mill, removing dust in tail gas by a spray granulator and a dryer, emptying, and preparing into the 15 percent clopyralid terbuthylazine dry suspending agent after passing the detection.
EXAMPLE 2318% Tripyric acid terbuthylazine wettable powder (1: 8)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 2% of clopyralid, 16% of terbuthylazine, TX-43%, DT-8006% and kaolin for the balance.
The process comprises the following steps: mixing the original medicine, the auxiliary agent and the filler according to the weight ratio, fully mixing and crushing by a jet mill, and preparing the 18 percent clopyralid terbuthylazine wettable powder after passing the detection.
Example 2412% Triton hydrochloride Water dispersible granules (1: 60)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 0.197 percent of clopyralid, 11.803 percent of terbuthylazine, SP-3011 percent, 2 percent of sodium lignosulfonate, 4 percent of diatomite and the balance of white carbon black.
The process comprises the following steps: taking the terbuthylazine raw drug and the clopyralid raw drug according to the formula, drying, weighing and crushing the terbuthylazine raw drug and the clopyralid raw drug, sequentially putting the terbuthylazine raw drug, the auxiliary agent and the filler into a preparation kettle in proportion, crushing and uniformly mixing the terbuthylazine raw drug, the auxiliary agent and the filler by a high-speed shearing machine, adding the binder and the water, uniformly mixing the mixture, granulating, drying and screening the mixture, and obtaining a finished product after quality inspection.
Example 2516% Triton Dichloropicolinic acid suspension (2: 1)
The weeding composition containing clopyralid and terbuthylazine comprises the following components: 10.67% of clopyralid, 5.33% of terbuthylazine, Morwet D-4253%, 0.2% of xanthan gum, 4% of ethylene glycol, 5002% of agricultural emulsion and water for balancing.
The process comprises the following steps: mixing the raw medicine, the auxiliary agent and water according to a weight ratio, uniformly mixing by a stirring kettle, performing high-speed shearing homogenization in a sand mill circulating sand mill and a high-shearing emulsification kettle, and preparing the 16% clopyralid-terbuthylazine suspending emulsion after passing detection.
Second, Effect test
I. Indoor combined action determination of clopyralid and terbuthylazine mixing
Purpose of the test
The combined action of the clopyralid and the terbuthylazine in the mixing process is determined by a bioassay test.
2 materials and methods:
the test is carried out in a greenhouse of the institute of grain and oil crops, academy of agriculture and forestry, Hebei province, according to the "NY/T1155.7-2006 indoor bioassay test criteria, part 7 of the herbicide: combined effect determination of compounding "in the Gowing method.
Target weeds were selected from common field weeds, large crabgrass (Digitaria sanguinalis L.), oryza sativa (Setariagenesis L.), Amaranthus retroflexus (Amaranthus retroflexus L.), and Cirsium japonicum (Cirsium japonicum DC.). The test agents were 96% clopyralid (clopyralid) and 97% terbuthylazine (terbuthylazine) on the market.
3/4 soil is added into a flowerpot with the diameter of 12cm, the soil is covered by 2mm after the weed seeds are sowed, and the medicine is taken when 2-4 leaves of the weed are planted.
Accurately weighing the original medicine by using a ten-thousandth electronic balance, respectively adding 2 times of N, N-dimethylformamide into the original medicine until the N, N-dimethylformamide is completely dissolved, and diluting with 0.1% of tween-80 aqueous solution to a constant volume. Then absorbing corresponding liquid medicine according to the liquid spraying amount, and spraying stems and leaves of the weeds by using an ASS-1 type spraying tower. The specific dosage of the medicament is shown in table 1.
The synergistic effect of the combination was evaluated using the Gowing method. Measuring the fresh weight of the overground part of the weeds at 14d after the application of the herbicide, and calculating the actual control effect (%) (blank control fresh weight-application treatment fresh weight) multiplied by 100% ÷ blank control fresh weight; the theoretical control effect (%) of the E0 mixture is E1+ E2 x (100-E1) ÷ 100, and E1 and E2 are the actual control effects of the corresponding single dose. The compound is an antagonistic action when the actual control effect E-theoretical control effect E0 is less than-5 percent, an additive action when the actual control effect E-theoretical control effect E0 is more than-5 percent, and a synergistic action when the actual control effect E-theoretical control effect E0 is more than 5 percent.
The agents and dose ratios set for each treatment are shown in table 1.
TABLE 1 clopyralid and terbuthylazine indoor combined action determination dosage meter (g ai/ha)
Figure BDA0002300057110000131
3 results of the test
Test results show that the control effect of the clopyralid on crab grass under different dosages is 2.7-21.6%, the control effect on green bristlegrass is 3.6-24.1%, the control effect on redroot amaranth is 18.7-81.6%, and the control effect on thistle is 62.5-95.2%; under different dosages of terbuthylazine, the control effect on crab grass is 41.5% -89.6%, the control effect on green bristlegrass is 46.7% -93.8%, the control effect on redroot amaranth is 62.8% -100%, and the control effect on circium japonicum is 22.5% -62.6% (table 2 and table 3).
Clopyralid and terbuthylazine in the formula (1-2): (1-60) the control effect on various weeds is obviously improved after the herbicide composition is mixed according to the weight proportion. The combined action test result shows that the combined action of the two on crab grass, green bristlegrass herb, redroot amaranth and Japanese thistle after the two are compounded is larger than zero, and the two are synergistic or additive (tables 2 and 3).
The combined action of the clopyralid and the terbuthylazine on 4 weeds after being mixed according to a certain proportion is synthesized in the following steps of (1-2): (1-24) the synergistic effect on weeds is strong in the proportion range.
TABLE 2 Combined action of clopyralid and terbuthylazine on crab and green bristlegrass after mixing
Figure BDA0002300057110000141
TABLE 3 Combined action of clopyralid and terbuthylazine on Amaranthus retroflexus and Cirsium japonicum after mixing
Figure BDA0002300057110000142
Figure BDA0002300057110000151
II. Clopyralid terbuthylazine herbicidal effect in field and influence on safety and quality of crops
1 purpose of the test:
the herbicidal effect, safety and influence on nutrient components (amino acid and fat) of the clopyralid terbuthylazine herbicidal composition are detected.
2 materials and methods:
the test agents were the herbicides prepared in examples 1, 2, 21; the control agent is a commercially available 75% clopyralid soluble granule, 50% terbuthylazine suspending agent, 57% 2, 4-D butyl ester missible oil and 38% atrazine suspending agent, the millet variety is Jigu T7, the broom corn millet variety is Jigu No. 2, and the test site is a test site on a levee of Ligusticum sinense city of Shijiazhuang in Hebei province.
The paddy field and the broom corn millet field are applied with the pesticide in the 2-5 leaf period of weeds and the 3-5 leaf period of crops in 7-16 months in 2019, the spraying amount is 40L/mu, the pesticide application instrument is an HD400 knapsack sprayer produced by Singapore Ringnong private company, and the sprayer is a fan-shaped sprayer. Measuring the fresh weight of the upper part of a 1 square meter of weeds every 30 days after the application of the herbicide, and calculating the fresh weight control effect of the herbicide on the weeds, wherein the calculation formula is as follows: the weed fresh weight control effect (%). times 100% of the weed fresh weight in the control area-the weed fresh weight in the application area/the weed fresh weight in the control area. And (4) measuring the yield of the millet and the broom corn millet in a cell during harvesting.
The amino acid content is determined by ninhydrin colorimetry, and the fat is determined by Soxhlet fat extractor.
Analysis of variance was performed using SPSS using a one-way random block method (Duncan for multiple comparison method).
3 results
The clopyralid terbuthylazine (examples 1, 2 and 21)500g ai/ha has good control effect on both gramineous weeds and dicotyledonous weeds in the field, and the total fresh weight control effect on the weeds 30 days after application is more than 95 percent, which is better than the control effect of the clopyralid terbuthylazine and terbuthylazine which are used separately. The results of the anova showed that the control effect of the herbicide in the case of 500g ai/ha in the examples 1, 2 and 21 was significantly different from that of clopyralid and terbuthylazine, and was significantly better than that of 2, 4-D butyl ester and atrazine, and was reduced by 33.3% compared with the terbuthylazine dosage (tables 4 and 5).
After 500g ai/ha of clopyralid terbuthylazine (examples 1, 2 and 21) of the ai/ha treatment agent, the crops grow normally and have no phytotoxicity symptoms, and the yield measurement result at harvest shows that the difference between the crop yield and the artificial weeding treatment is not significant and is obviously better than that of the contrast agent and the clear water (tables 6 and 7). The crops such as corn, soybean, peanut, cotton and the like around the crops are observed by eyes to grow normally without phytotoxicity symptoms. After the 57% 2, 4-D butyl ester emulsifiable solution is applied, the nearby leaves of soybeans and cotton have a wrinkle phenomenon.
Post-harvest quality measurements of the crops showed that the products of the invention (examples 1, 2, 21) significantly increased the levels of the major nutrients amino acids and fats compared to the control (table 6, table 7).
TABLE 4 herbicidal composition of clopyralid terbuthylazine against weeds in paddy field
Note that the difference was not significant at the level of α -0.05 for the same letter and at the level of α -0.05 for the different letter in the table, which is the same as the table below.
TABLE 5 herbicidal Effect of clopyralid terbuthylazine on Panicum miliaceum weeds
Figure BDA0002300057110000172
TABLE 6 influence of the Agents on millet yield and quality
Figure BDA0002300057110000181
TABLE 7 Effect of agents on broom corn millet yield and quality

Claims (8)

1. A weeding composition containing clopyralid and terbuthylazine is characterized by comprising 10-90% of active ingredients, the balance of auxiliaries and carriers in percentage by weight, wherein the active ingredients comprise (1-2): (1-60) clopyralid and terbuthylazine.
2. The herbicidal composition containing clopyralid and terbuthylazine as claimed in claim 1, wherein the weight ratio of the active ingredients is (1-2): (2-24) clopyralid and terbuthylazine.
3. The herbicidal composition containing clopyralid and terbuthylazine as claimed in claim 1, wherein said active ingredients are present in a weight ratio of 1: 8 and terbuthylazine.
4. The herbicidal composition as claimed in claim 1, wherein the adjuvant is one or more selected from the group consisting of safeners, wetting agents, dispersants, binders, emulsifiers, and penetrants.
5. The herbicidal composition of claim 4, wherein the safener is selected from the group consisting of CGA-28725, CGA-145138, chloranilide, isoxadifen, cyprosulfamide, R-25788, MG-191, cloquintocet, gibberellin, 1, 8-naphthalic anhydride, brassinolide, CGA-154281, Hoe-70542, clethodim, benzyl 2-chloro-4-trifluoromethyl-1, 3-thiazole-5-carboxylate, dichloroacetyl diisopropylamine, 3-dichloroacetyl-5- (2-furyl) -2, 2-dimethyl-1, 3-oxazolidine, mefenpyr, and antidote T.
6. The herbicidal composition containing clopyralid and terbuthylazine as claimed in claim 1, wherein said composition is one of suspending agent, dry suspending agent, wettable powder, water dispersible granule and suspoemulsion.
7. The use of a herbicidal composition comprising clopyralid and terbuthylazine as claimed in claim 1, wherein the herbicidal composition is used for foliar treatment after emergence in crop fields.
8. The use of the herbicidal composition comprising clopyralid and terbuthylazine as claimed in claim 7, wherein said crop fields include millet fields and broom corn fields.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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