CN115104622A - Compound composition of refined glufosinate-ammonium and topramezone - Google Patents

Compound composition of refined glufosinate-ammonium and topramezone Download PDF

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CN115104622A
CN115104622A CN202110301230.1A CN202110301230A CN115104622A CN 115104622 A CN115104622 A CN 115104622A CN 202110301230 A CN202110301230 A CN 202110301230A CN 115104622 A CN115104622 A CN 115104622A
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compound composition
ammonium
topramezone
glufosinate
mass
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CN115104622B (en
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赵辉
陈根宝
凌江涛
钱海宾
沈建良
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Jiangsu Qizhou Green Technology Research Institute Co ltd
Jiangsu Sevencontinent Green Chemical Co Ltd
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Jiangsu Qizhou Green Technology Research Institute Co ltd
Jiangsu Sevencontinent Green Chemical 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
    • A01N57/00Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
    • A01N57/18Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
    • A01N57/20Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals
    • 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

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

Abstract

The invention relates to a compound composition of refined glufosinate-ammonium and topramezone, which comprises active ingredients, wherein the active ingredients comprise the refined glufosinate-ammonium and the topramezone in a mass ratio of 0.01-100: 1. The components of the invention have good synergy and synergism, can be effectively used for preventing and treating perennial tolerant plants, old weeds and the like, effectively improves the prevention and treatment range of glufosinate-ammonium and topramezone, and obviously prolongs the lasting period. Meanwhile, the preparation method of the composition is simple and easy to implement, the processing equipment is easy to obtain, the cost is low, and the market popularization value and the economic benefit are obvious.

Description

Compound composition of refined glufosinate-ammonium and topramezone
Technical Field
The invention belongs to the field of application of agricultural chemicals, and particularly relates to a compound composition of refined glufosinate-ammonium and topramezone.
Background
The chemical formula of the refined glufosinate-ammonium is C 5 H 12 NO 4 P has a formula weight of 181.27 and a chemical name of 4- [ hydroxy (methyl) phosphono group]The L-homoalanine is easy to dissolve in water, difficult to dissolve in an organic solvent, stable to light, has a melting point of 214 ℃ and 216 ℃, and is a high-efficiency, low-toxicity and non-selective contact-type phosphoric acid herbicide. The refined glufosinate-ammonium is L-type glufosinate-ammonium, which has twice the herbicidal activity of the racemic DL-type glufosinate-ammonium mixture. The glufosinate-ammonium inhibits glutamine synthetase, so that nitrogen metabolism disorder in plants is caused, ammonium ion accumulation poisoning is caused, chloroplast synthesis is further influenced, photosynthesis is hindered, and finally, the plants die. The glufosinate-ammonium is low in toxicity, safe, easy to degrade in soil, safe to crops, wide in weeding spectrum, high in activity, quick in weeding, capable of preventing and killing or quickly killing 100 kinds of annual or perennial weeds, mainly in contact weeding, not transferred to other places, and safe to succeeding crops. The refined glufosinate-ammonium has good water solubility and stable structure, and is convenient to process and mix for use.
Topramezone has the chemical formula C 16 H 17 N 3 O 5 S, formula weight is 363.38, chemical name is 4- [3- (4, 5-dihydroisoxazol-3-yl) -2-methyl-4-methylsulfonyl]-1-methyl-5-hydroxy-1H-pyrazole, a highly selective post-emergence herbicide for corn fields. A herbicide in the form of 4-Hydroxy Phenyl Pyruvate Dioxygenase (HPPD) as herbicide for preventing and eliminating annual gramineous and latifolious weeds, such as crab grass, green bristlegrass, etc is prepared from the 4-Hydroxy Phenyl Pyruvate Dioxygenase (HPPD) as inhibitor, which can be absorbed by root system and part of plant and conducted upward and downward in plant body.
The biological activities of different herbicides are different, the weed control spectra are different, the combination can play a good complementary and synergistic effect theoretically, and particularly, the combination of the herbicides with different action mechanisms and modes is carried out. However, in practical application, it is found that the synergistic effect can be achieved by not compounding any herbicide, and the complementary effect is related to not only compounding of different herbicides but also formulation of the composition and other ingredients, but few researches and reports on compounding of glufosinate-ammonium and topramezone are provided at present.
Disclosure of Invention
The invention aims to provide a compound composition of glufosinate-ammonium and topramezone for controlling the growth of vegetation which does not want to grow and gaining control effect.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a compound composition of refined glufosinate-ammonium and topramezone, which comprises active ingredients, wherein the active ingredients comprise the refined glufosinate-ammonium and the topramezone in a mass ratio of 0.01-100: 1.
Preferably, the mass ratio of the refined glufosinate-ammonium to the topramezone is 1-50: 1.
further preferably, the mass ratio of the glufosinate-ammonium to the topramezone is 5-20: 1.
preferably, the mass of the active ingredient is 10-85% of the total weight of the compound composition.
Preferably, the compound composition also comprises an auxiliary material, wherein the auxiliary material comprises a surfactant accounting for 5-20% of the total weight of the compound composition.
The surfactant is one or more selected from wetting agent, emulsifier and dispersant.
Further preferably, the surfactant is one or more selected from fatty alcohol-polyoxyethylene ether, tallow amine-polyoxyethylene ether, alkyl glycoside, alkylbenzene sulfonate, alkyl sulfate, polycarboxylate, sodium lignosulfonate and organic silicon.
Further preferably, the auxiliary materials further comprise one or more of a combination of an antifreezing agent, a solvent, a filler, a disintegrating agent, an antifoaming agent, a binder and a pigment.
The antifreezing agent is one or more of glycerol, propylene glycol and ethylene glycol;
the solvent is one or a combination of more of water, ethanol, methanol, N-dimethylformamide, dimethyl sulfoxide, cyclohexanone, methyl oleate and soybean oil;
the filler is one or a combination of more of diatomite, kaolin, bentonite, white carbon black and light calcium carbonate;
the disintegrating agent is one or more of ammonium sulfate, urea, polyvinylpyrrolidone, sodium sulfate, starch and its derivatives, cellulose, sodium bicarbonate, sodium lauryl sulfate, sodium alginate, bentonite, and sodium chloride;
the adhesive is one or more of starch, gelatin, pregelatinized starch, acacia, polyvinylpyrrolidone, methylcellulose, hydroxypropyl methylcellulose, polyethylene glycol, polyvinyl alcohol, glucose and sucrose.
Preferably, the formulation of the compound composition of glufosinate-ammonium and topramezone is soluble liquid, suspending agent, suspoemulsion, oil suspending agent, soluble powder, soluble granule, wettable powder or water dispersible granule.
According to one embodiment, the compound composition of the refined glufosinate-topramezone comprises the following components in percentage by mass:
10 to 60 percent of active component;
5 to 20 percent of surfactant;
35 to 75 percent of solvent.
According to another embodiment, the compound composition of the refined glufosinate-topramezone comprises the following components in percentage by mass:
30 to 85 percent of active component;
5 to 10 percent of surfactant;
10 to 60 percent of filler.
Preferably, the formulation of the compound composition of glufosinate-ammonium and topramezone is soluble liquid, suspending agent, oil suspending agent, soluble powder, soluble granule, wettable powder or water dispersible granule.
Preferably, when the compound composition is a soluble liquid, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000031
further preferably, when the compound composition is a soluble liquid agent, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000032
further preferably, when the compounded composition is a soluble liquid, the solvent is water, and the surfactant is alkyl glycoside.
The preparation method of the compound combination with the dosage form of soluble liquid comprises the following steps:
adding refined glufosinate-ammonium and topramezone into a solvent, stirring and dissolving at the temperature of 55-65 ℃ at the speed of 150-200 rpm, then adding other auxiliary materials, uniformly stirring, and cooling to room temperature to obtain a soluble liquid of the compound composition of the refined glufosinate-ammonium and the topramezone.
Preferably, when the compound composition is a suspending agent, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000033
further preferably, when the compound composition is a suspending agent, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000034
further preferably, when the compound composition is a suspending agent, the solvent is water, and the surfactant is fatty alcohol-polyoxyethylene ether and/or polycarboxylate.
Preferably, when the compound composition is an oil suspending agent, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000041
further preferably, when the compound composition is an oil suspending agent, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000042
further preferably, when the compound composition is an oil suspending agent, the solvent is methyl oleate, and the surfactant is fatty alcohol-polyoxyethylene ether and/or alkylbenzene sulfonate.
The preparation method of the compound composition with the dosage form of the suspending agent or the oil suspending agent comprises the following steps:
adding refined glufosinate-ammonium, topramezone and auxiliary materials into a solvent, uniformly stirring at the speed of 150-200 revolutions per minute, and grinding by a sand mill to obtain a suspending agent or oil suspending agent of the compound composition of the refined glufosinate-ammonium and the topramezone.
Preferably, when the compound composition is soluble powder, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000043
further preferably, when the compound composition is soluble powder, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000044
further preferably, when the compound composition is soluble powder, the surfactant is alkylbenzene sulfonate, and the filler is kaolin and/or diatomite.
Preferably, when the compound composition is a soluble granule, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000045
further preferably, when the compound composition is a soluble granule, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000051
further preferably, when the compounded composition is a soluble powder, the surfactant is an alkyl sulfate and/or a polycarboxylate.
Preferably, when the compound composition is wettable powder, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000052
further preferably, when the compound composition is wettable powder, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000053
further preferably, when the compounded composition is a wettable powder, the surfactant is a polycarboxylate.
The preparation method of the compound composition with the dosage form of the suspending agent or the oil suspending agent comprises the following steps:
the refined glufosinate-ammonium, the topramezone and the auxiliary materials are uniformly stirred and are subjected to superfine grinding through a jet mill to prepare soluble powder or wettable powder of the compound composition of the refined glufosinate-ammonium and the topramezone.
Preferably, when the compound composition is a water dispersible granule, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000054
further preferably, when the compound composition is a water dispersible granule, the compound composition comprises the following components in percentage by mass:
Figure BDA0002986344290000055
further preferably, when the compounded composition is a water dispersible granule, the surfactant is polycarboxylate and/or lignosulfonate, and the filler is kaolin.
The preparation method of the compound composition with the dosage form of soluble granules or water dispersible granules comprises the following steps:
stirring and uniformly mixing the refined glufosinate-ammonium, the topramezone and the auxiliary materials, carrying out superfine grinding through a jet mill, adding water, kneading in a kneading machine, then extruding and granulating in an extrusion granulator, and drying to obtain the soluble granules or the water dispersible granules of the compound composition of the refined glufosinate-ammonium and the topramezone.
The compound composition of the refined glufosinate-ammonium and the topramezone can solve the problems that the existing herbicide cannot completely prevent and control field tolerant weeds, resistant weeds and old weeds, is short in lasting period and needs to be repeatedly applied for many times. The invention takes the refined glufosinate-ammonium and the topramezone as active ingredients, the active ingredients are mixed in a certain range, the synergistic weeding effect of the active ingredients is fully exerted under the coordination of other components of the preparation, the drug effect is obviously superior to that of the refined glufosinate-ammonium and the topramezone which are used independently, and meanwhile, the compound composition of the refined glufosinate-ammonium and the topramezone is simple, convenient and feasible, has stable product quality, obvious market value and is suitable for large-scale popularization and application.
The compound composition of the glufosinate-ammonium and the topramezone is used for preventing and controlling the growth of vegetation which is not expected to grow, and comprises weed control in non-cultivated fields, forest weeding, orchard weeding, inter-row weeding of crops in cultivated fields, and field stubble cleaning before sowing or transplanting.
When the composition is used, the effective component dosage of the compound composition of the refined glufosinate-ammonium and the topramezone is 115-1150 g/ha.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
the components of the invention have good synergy and synergism, can be effectively used for preventing and treating perennial tolerant plants, old weeds and the like, effectively improves the prevention and treatment range of glufosinate-ammonium and topramezone, and obviously prolongs the lasting period. Meanwhile, the preparation method of the composition is simple and easy to implement, the processing equipment is easy to obtain, the cost is low, and the market popularization value and the economic benefit are obvious.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations where mutually exclusive features or steps are expressly stated.
The invention will now be further described with reference to specific examples, but the invention should not be limited to these examples, but may be substituted by other equivalent or similarly purposed alternative features unless specifically stated. Unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features. The contents are all mass contents, and "%" is mass percent.
The glufosinate-ammonium is purchased from Zhejiang Yongnong chemical industries, Ltd; topramezone is available from basf european corporation; the fatty alcohol-polyoxyethylene ether is purchased from the petroleum chemical plant of Haian of Jiangsu province; alkyl glycosides were purchased from Shanghai Kai chemical Co., Ltd; the alkylbenzene sulfonate is purchased from Shanghai Zhongzhong fine chemical industry Co., Ltd; alkyl sulfates were purchased from steganochemical (shanghai) ltd; polycarboxylates are available from Shandongtai and Water treatment science and technology Co., Ltd; sodium lignosulfonate was purchased from jinbao agro-chemical technology ltd, yang, vortex county; the antifoaming agent is purchased from break-Thai chemical Co., Ltd of Nantong city; polyethylene glycol was purchased from Haian petrochemical plants of Jiangsu province; methylcellulose is available from Shanghai Merlin Biotech, Inc.; kaolin was purchased from Shanghai Guo research industries, Inc.; diatomaceous earth was purchased from Shanghai Mingsheng industries, Inc.; bentonite was purchased from Guangxi Runxing New materials, Inc.; mesotrione was purchased from Zhongshan chemical Co., Ltd, Anhui; cycliophenones were purchased from bayer ag; isoxaflutole is available from bayer ag.
Example 1
Weed activity determination test report by mixing refined glufosinate-ammonium and topramezone
The purpose of the test is as follows: the weeding effect of the mixing of the glufosinate-ammonium and the topramezone on the target weeds is measured under the greenhouse potting condition, and the combined action of the glufosinate-ammonium and the topramezone is evaluated.
Test targets: green bristlegrass herb, large crabgrass herb, purslane and abutilon.
Preparing a test material: the test soil was dosed at 4/5 to the bowl. The mode of infiltrating irrigation at the bottom of the pot is adopted, so that the soil is completely wet. Uniformly sowing the weed seeds to be tested which are subjected to the pre-treatment for accelerating germination to expose white on the surface of the soil, covering a small amount of soil according to the size of the seeds, transferring the seeds into a greenhouse for conventional culture after sowing, and supplementing water in a mode of infiltrating irrigation at the bottom of a pot. Planting after emergence and before application, 5 purslane and piemarker plants per pot, and 10 crab grass and green bristlegrass plants per pot.
The proportioning design of medicament compounding: the test shows that the weed control spectra and the action modes of the two agents are complementary, so that the compounding test adopts a Gowing method, and the compounding ratio is shown in a table 1 (unit: g.a.i/ha).
TABLE 1
Figure BDA0002986344290000071
Treating a medicament: according to the action characteristics and the medicament mixing purpose of the medicament, a stem leaf spraying method is adopted for the test reference of pesticide bioassay technology (edited by Chennian spring Sunday and published by Beijing agriculture university Press) and agricultural industry standard of the people's republic of China (herbicides NY/T1155.3-2006 and 1155.4-2006 in pesticide indoor bioassay test guidelines). The prepared potted weeds are placed in a spraying tower, and are sprayed quantitatively by a rotary disc under the constant pressure of 0.4MPA and 10ml of spraying liquid medicine (the amount of the liquid medicine is 33Kg per mu) for settling for 1 minute. Each treatment was repeated 4 times, with 3 pots per grass repeat. After the surface of the treated material is naturally air-dried, the material is placed at 18-25 ℃ and managed according to the conventional method, and water is supplemented in an infiltrating irrigation mode at the bottom of the pot.
The investigation method comprises the following steps: shearing off the overground part of the weeds 14 days after the application of the herbicide, and weighing the fresh weight; and calculating the fresh weight control effect. While the symptoms of the injury were recorded. Such as: color change (yellowing, whitening, etc.); morphological changes (malformation of heart lobes, distortion); growth changes (dehydration, wilting, dwarfing, clumping, etc.).
Data statistics and analysis: the two groups of medicaments have strong complementarity, are treated by a Gowing method, and calculate the fresh weight control effect (percentage, percent) according to a formula (1).
E=(C-T)*100/C…………………………(1)
In the formula: e, fresh weight control effect; c, comparing the fresh weight of the overground part of the weed; and T, treating the fresh weight of the overground part of the weed.
The theoretical control effect of the two agents is calculated according to the formula (2).
Figure BDA0002986344290000081
In the formula:
x- - -weed control effect when the dosage of the herbicide A is P;
y- - -weed control effect when the dosage of the herbicide B is Q;
E 0 theoretical control when the amount of herbicide a is P and the amount of herbicide B is Q;
e- - -the actual control effect when the dosage of the herbicide A is P and the dosage of the herbicide C is Q;
E-E 0 the synergistic effect is more than 10 percent; E-E 0 The antagonism is less than-10 percent; E-E 0 Has a value between+10% is addition.
The results of the weed activity measurements of the combination of glufosinate-ammonium and topramezone are shown in table 2.
TABLE 2
Figure BDA0002986344290000082
Figure BDA0002986344290000091
As can be seen from Table 2, the use of glufosinate-ammonium and topramezone alone is effective in inhibiting weed growth only at high doses. After compounding, the pesticide effect of the indoor potted plants is obviously improved under different compounding proportions, and all treatments are E-E 0 The values are all > -10%, and the combined evaluation shows obvious synergistic or additive effect.
From the observation of the weeds after the application, 3d after the application, the weeds subjected to compound treatment have the symptoms of glufosinate-ammonium poisoning, then gradually spread and necrotize, and the phytotoxicity symptoms of various weeds are more obvious along with the increase of the dosage. After 5 days of application, the compound treatment of the weeds has topramezone poisoning symptoms such as whitish leaves and inhibited growth, the compound combination treatment effect in different proportions is obviously better than that of each single agent, and the action speed is obviously faster than that of the single agent.
Example 2
10% of refined glufosinate-ammonium + 0.5% of topramezone soluble liquor is prepared, and the raw material formula is shown in table 3.
TABLE 3
Components Proportioning
Refined glufosinate-ammonium 10% folding
Topramezone 0.5% folding
Surfactant alkyl glycoside 12%
Defoaming agent 0.1%
Antifreeze ethylene glycol 5%
Water (W) Make up to 100%
Adding refined glufosinate-benzoxadim into water to dissolve, keeping the temperature at 60 ℃, stirring at 180 revolutions per minute until the original drug is completely dissolved, adding a defoaming agent and a surfactant alkyl glycoside, uniformly stirring, and cooling to room temperature to obtain a 10.5% refined glufosinate-benzoxadim soluble liquid.
Example 3
A suspension of 40% refined glufosinate-ammonium + 8% topramezone was prepared, the raw material formulation of which is given in table 4.
TABLE 4
Components Proportioning
Refined glufosinate-ammonium 40% Baibiao
Topramezone 8% folding
Fatty alcohol polyoxyethylene ether as surfactant 4%
Surfactant polycarboxylates 4%
Propylene glycol as antifreezing agent 5%
Water (W) Make up to 100%
Adding refined glufosinate-benzoxadim and a surfactant into water, stirring at 180 revolutions per minute until the raw pesticide is wetted and dissolved, and sanding by a sanding machine to obtain the 48% refined glufosinate-benzoxadim suspending agent.
Example 4
24% of glufosinate-ammonium and 8% of topramezone oil suspending agent are prepared, and the raw material formula is shown in table 5.
TABLE 5
Components Proportioning
Refined glufosinate-ammonium 24% o
Topramezone 8% folding
Fatty alcohol polyoxyethylene ether as surfactant 12%
Surface active agentAlkyl benzene sulfonate 6%
Bentonite clay 2%
Oleic acid methyl ester Make up to 100%
Adding refined glufosinate-benzoxadim, bentone and a surfactant into methyl oleate, stirring at 180 revolutions per minute until the technical material is wet, and sanding by a sanding machine to obtain the 32% refined glufosinate-benzoxadim oil suspending agent.
Example 5
A 40% refined glufosinate-ammonium + 8% topramezone soluble powder was prepared, the raw material formulation of which is shown in table 6.
TABLE 6
Figure BDA0002986344290000101
Figure BDA0002986344290000111
And uniformly stirring and mixing the refined glufosinate-ammonium, the topramezone, the surfactant alkylbenzene sulfonate, the polyethylene glycol and the filler according to the proportion, and carrying out superfine grinding by using a jet mill to obtain 48% of refined glufosinate-topramezone soluble powder.
Example 6
36% refined glufosinate-ammonium + 6% topramezone soluble granules were prepared, and the raw material formulation thereof is shown in table 7.
TABLE 7
Components Proportioning
Refined glufosinate-ammonium 36% Bailian (Chinese character of 'Bailian')
Topramezone 6% Bailian
Surfactant alkyl sulfates 3.5%
Surfactant polycarboxylates 4%
Disintegrating agent ammonium sulfate 5%
Filler diatomite Make up to 100%
And uniformly stirring and mixing the refined glufosinate-ammonium, the topramezone, the surfactant, the disintegrating agent and the filler according to the proportion, carrying out superfine grinding by using a jet mill, adding 9% of water, kneading for 20 minutes in a kneading machine, extruding and granulating in an extrusion granulator, and drying for 30 minutes at 60 ℃ to obtain the 42% refined glufosinate-topramezone soluble granules.
Example 7
60% of refined glufosinate-ammonium + 10% of topramezone wettable powder is prepared, and the raw material formula is shown in table 8.
TABLE 8
Components Proportioning
Refined glufosinate-ammonium 60% Baibiao
Topramezone 10% folding
Surfactant polycarboxylates 5%
Adhesive polyethylene glycol 2%
Filler kaolin Make up to 100%
The refined glufosinate-benzoxadim wettable powder is prepared by uniformly stirring and mixing the refined glufosinate, the topramezone, the surfactant, the polyethylene glycol and the filler according to the proportion and carrying out superfine grinding by a jet mill.
Example 8
30% of refined glufosinate-ammonium and 6% of topramezone water dispersible granules are prepared, and the raw material formula is shown in table 9.
TABLE 9
Components Proportioning
Refined glufosinate-ammonium 30% of the total weight
Glyphosate 6% folding
Surfactant polycarboxylates 3%
Surfactant lignosulfonate 3%
Adhesive methylcellulose 1%
Filler kaolin Make up to 100%
And uniformly stirring and mixing the refined glufosinate-ammonium, the topramezone, the surfactant, the adhesive and the filler according to the proportion, carrying out superfine grinding by a jet mill, adding 13% of water for kneading and granulating, adding into an extrusion granulator for extrusion granulation, and drying at 60 ℃ to obtain the 36% refined glufosinate-topramezone water dispersible granule.
Comparative example 1
A 40% refined glufosinate-ammonium + 8% topramezone soluble powder (no polyethylene glycol, kaolin, as compared to example 5) was prepared according to the raw material formulation shown in table 10.
Watch 10
Components Proportioning
Refined glufosinate-ammonium 40% Baibiao
Topramezone 8% folding
Surfactant alkyl benzene sulfonate 5%
Filler diatomite Make up to 100%
And uniformly stirring and mixing the refined glufosinate-benzoxadim, the surfactant alkyl benzene sulfonate and the filler according to the proportion, and carrying out superfine grinding by using a jet mill to obtain 48% of refined glufosinate-benzoxadim soluble powder.
Comparative example 2
A 40% refined glufosinate-ammonium + 8% topramezone suspension (no fatty alcohol-polyoxyethylene ether as compared to example 3) was prepared, the raw material formulation of which is shown in table 11.
TABLE 11
Figure BDA0002986344290000121
Figure BDA0002986344290000131
Adding refined glufosinate-ammonium, topramezone and polycarboxylate into water, stirring at 180 revolutions per minute until the original drug is wetted and dissolved, and sanding by a sand mill to obtain the 48% refined glufosinate-topramezone suspending agent.
Comparative example 3
A suspension concentrate of 40% glufosinate-ammonium + 8% mesotrione (compared to example 3, the active ingredient topramezone was replaced by mesotrione, the remaining ingredients being the same) was prepared and the raw material formulation is as shown in table 12.
TABLE 12
Components Proportioning
Refined glufosinate-ammonium 40% Baibiao
Mesotrione 8% Bailian
Fatty alcohol polyoxyethylene ether as surfactant 4%
Surfactant polycarboxylates 4%
Antifreezing agent propylene glycol 5%
Water (W) Make up to 100%
Adding refined glufosinate-ammonium, mesotrione and a surfactant into water, stirring at 180 r/min until the raw materials are wetted and dissolved, and sanding by a sanding machine to obtain the 48% refined glufosinate-mesotrione suspending agent.
Comparative example 4
A suspension of 40% glufosinate-ammonium + 8% tembotrione (compared to example 3, the active ingredient topramezone was replaced by tembotrione, the remaining ingredients were the same) was prepared according to the raw material formulation shown in table 13.
Watch 13
Components Proportioning
Refined glufosinate-ammonium 40% Bailian
Cyclosultone 8% folding
Fatty alcohol polyoxyethylene ether as surfactant 4%
Surfactant polycarboxylates 4%
Antifreezing agent propylene glycol 5%
Water (W) Make up to 100%
Adding refined glufosinate-ammonium, tembotrione and a surfactant into water, stirring at 180 revolutions per minute until the original drug is wetted and dissolved, and sanding by a sand mill to prepare the 48 percent refined glufosinate-tembotrione suspending agent.
Comparative example 5
A suspension of 40% glufosinate-ammonium + 8% isoxaflutole (the active ingredient topramezone was replaced with isoxaflutole and the remaining ingredients were the same as in example 3) was prepared according to the raw material formulation shown in table 14.
TABLE 14
Components Proportioning
Refined glufosinate-ammonium 40% Baibiao
Isoxaflutole 8% folding
Fatty alcohol polyoxyethylene ether as surfactant 4%
Surfactant polycarboxylates 4%
Propylene glycol as antifreezing agent 5%
Water (W) Make up to 100%
Adding refined glufosinate-ammonium, isoxaflutole and a surfactant into water, stirring at 180 revolutions per minute until the original drug is wetted and dissolved, and sanding by a sanding machine to obtain the 48% refined glufosinate-isoxaflutole suspending agent.
Example 9
The purpose of the test is to confirm the actual control effect of the compound preparation of the glufosinate-ammonium and the imazamox on the weeds in the corn field, to comprehensively evaluate the compound of the glufosinate-ammonium and the topramezone, and to provide a certain theoretical basis for the next specific application. The test is executed according to the GB/T17980-.
1 materials and methods
1.1 test agent
The control agent is a compound preparation of refined glufosinate-ammonium, topramezone and the like, and is specifically shown in examples 2-8 and comparative examples 1-5.
A contrast medicament of 10 percent of refined glufosinate-ammonium aqueous solution (purchased from the market) and 30 percent of topramezone suspending agent (purchased from the market).
1.2 test subjects
The weeds in the corn field mainly comprise barnyard grass, green bristlegrass, crab grass, purslane and acalypha australis, and the perennial weeds mainly comprise horseweed herb and polygonum cuspidatum. When the herbicide is applied, the coverage of weeds in each treatment plot is 80%, and the plant heights are different from 15 cm to 30 cm.
1.3 design of the experiment
The experiment was set with 14 treatments and each was set with a blank control treatment (CK) of 66 square meters per cell area, 3 replicates for a total of 45 cells. The cells for different treatments were arranged in completely random blocks. The design process is shown in Table 15.
Watch 15
Processing number Treatment agent The dosage of effective component (g/mu)
A Example 2 25
B Example 3 25
C Example 4 25
D Example 5 25
E Example 6 25
F Example 7 25
G Example 8 25
H Comparative example 1 25
I Comparative example 2 25
J Comparative example 3 25
K Comparative example 4 25
L Comparative example 5 25
M 10% refined glufosinate solution (drug control) 25
N 30% topramezone suspending agent (control) 4
O Blank (CK) /
1.4 test environmental conditions
The test place is Anyizhen in Baoxingcounty in Jiangsu province, the upper crop in the test field is wheat, the wheat crop is higher, and the height of the corn plant is about 30 cm. The test field has flat condition and sandy loam.
And (4) test weather: the medicine is cloudy in the day of application, the highest air temperature is 32 ℃, the lowest air temperature is 24 ℃, and no wind exists. There was rainfall 5 days after dosing.
1.5 test methods
The test is carried out in 12 am 7/month in 2020, the backpack electric sprayer is used for spraying, the protective cover is installed, the directional spraying is carried out on weeds among corn rows, and the liquid medicine is prevented from being sprayed to the corn by 30L/mu of each treatment water as far as possible.
2 investigation method and drug efficacy evaluation method
The control effect of each treatment was investigated at 10d and 21d after the application, and the species and the number of the weeds were recorded by taking 0.5 square meter of each spot by 3-spot sampling. The effect on corn was also visually observed.
Figure BDA0002986344290000151
The results of the investigation are shown in Table 16 below.
TABLE 16
Figure BDA0002986344290000161
As can be seen from Table 16, compared with the comparative examples and the control agents, the control effects of the refined glufosinate-ammonium and topramezone on annual and perennial weeds in fields of different examples are obviously improved, the control effects on annual and perennial weeds in the fields are higher than 80% in 10 days, and the control effects on annual and perennial weeds in 21 days are higher than 80%.
Although the comparative examples 1 and 2 are also the compound of the refined glufosinate-ammonium and the topramezone, the selection of the surfactant, the filler and the like is unreasonable, the control effect in 10 days and 21 days is lower than 75 percent, the control effect is obviously lower than the effects of the corresponding examples 5 and 3, and the components and the proportion selected in the examples are more reasonable.
Compared with the comparative example 3, the comparative example 4 and the comparative example 5, the effective component topramezone in the example 3 is replaced by mesotrione, tembotrione and isoxaflutole with similar structures and action modes respectively, the control effect is lower than 70% in 10 days and 21 days, and the compounding of the three components and the refined glufosinate-ammonium is not obvious in synergistic effect compared with the compounding of the refined glufosinate-ammonium and topramezone.
The treated corns grow normally and are safe to the corns.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (10)

1. A compound composition of refined glufosinate-ammonium and topramezone is characterized in that: the composition comprises active ingredients, wherein the active ingredients comprise refined glufosinate-ammonium and topramezone in a mass ratio of 0.01-100: 1.
2. The compound composition of glufosinate-ammonium and topramezone according to claim 1, which is characterized in that: the mass ratio of the refined glufosinate-ammonium to the topramezone is 1-50: 1.
3. the compound composition of refined glufosinate-ammonium and topramezone according to claim 2, characterized in that: the mass ratio of the refined glufosinate-ammonium to the topramezone is (5-20): 1.
4. the combination composition of refined glufosinate and topramezone according to any one of claims 1 to 3, characterized in that: the mass of the active component is 10-85% of the total weight of the compound composition.
5. The combination composition of refined glufosinate and topramezone according to any one of claims 1 to 3, characterized in that: the compound composition also comprises auxiliary materials, wherein the auxiliary materials comprise a surfactant accounting for 5-20% of the total weight of the compound composition, and the surfactant is one or a combination of a wetting agent, an emulsifying agent and a dispersing agent.
6. The compound composition of refined glufosinate-ammonium and topramezone according to claim 5, characterized in that: the surfactant is one or more of fatty alcohol-polyoxyethylene ether, tallow amine-polyoxyethylene ether, alkyl glycoside, alkylbenzene sulfonate, alkyl sulfate, polycarboxylate, sodium lignosulfonate and organic silicon.
7. The compound composition of glufosinate-ammonium and topramezone according to claim 5, which is characterized in that: the auxiliary materials also comprise one or more of antifreeze, solvent, filler, disintegrating agent, defoaming agent, adhesive and pigment;
the antifreezing agent is one or more of glycerol, propylene glycol and ethylene glycol;
the solvent is one or a combination of more of water, ethanol, methanol, N-dimethylformamide, dimethyl sulfoxide, cyclohexanone, methyl oleate and vegetable oil;
the filler is one or a combination of more of diatomite, kaolin, bentonite, white carbon black and light calcium carbonate;
the disintegrating agent is one or more of ammonium sulfate, urea, polyvinylpyrrolidone, sodium sulfate, starch and its derivatives, cellulose, sodium bicarbonate, sodium lauryl sulfate, sodium alginate, bentonite, and sodium chloride;
the adhesive is one or more of starch, gelatin, pregelatinized starch, acacia, polyvinylpyrrolidone, methylcellulose, hydroxypropyl methylcellulose, polyethylene glycol, polyvinyl alcohol, glucose and sucrose.
8. The compound composition of refined glufosinate-ammonium and topramezone according to claim 1, characterized in that: the compound composition of the refined glufosinate-ammonium and the topramezone comprises the following components in percentage by mass:
10 to 60 percent of active component;
5 to 20 percent of surfactant;
35 to 75 percent of solvent.
9. The compound composition of glufosinate-ammonium and topramezone according to claim 1, which is characterized in that: the compound composition of the refined glufosinate-ammonium and the topramezone comprises the following components in percentage by mass:
30 to 85 percent of active component;
5 to 10 percent of surfactant;
10 to 60 percent of filler.
10. The compound composition of glufosinate-ammonium and topramezone according to claim 1, which is characterized in that: the formulation of the compound composition of glufosinate-ammonium and topramezone is soluble liquid, suspending agent, oil suspending agent, soluble powder, soluble granules, wettable powder or water dispersible granules;
when the compound composition is a soluble liquid, the compound composition comprises the following components in percentage by mass:
Figure FDA0002986344280000021
when the compound composition is a suspending agent, the compound composition comprises the following components in percentage by mass:
Figure FDA0002986344280000022
when the compound composition is an oil suspending agent, the compound composition comprises the following components in percentage by mass:
Figure FDA0002986344280000023
when the compound composition is soluble powder, the compound composition comprises the following components in percentage by mass:
Figure FDA0002986344280000024
when the compound composition is a soluble granule, the compound composition comprises the following components in percentage by mass:
Figure FDA0002986344280000025
Figure FDA0002986344280000031
when the compound composition is wettable powder, the compound composition comprises the following components in percentage by mass:
Figure FDA0002986344280000032
when the compound composition is a water dispersible granule, the compound composition comprises the following components in percentage by mass:
Figure FDA0002986344280000033
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