CN117256622A

CN117256622A - Compound herbicide containing glufosinate-ammonium

Info

Publication number: CN117256622A
Application number: CN202311258744.9A
Authority: CN
Inventors: 沈建良; 梁江涛; 钱海宾; 安静
Original assignee: Jiangsu Sevencontinent Green Chemical Co Ltd
Current assignee: Jiangsu Sevencontinent Green Chemical Co Ltd
Priority date: 2023-09-27
Filing date: 2023-09-27
Publication date: 2023-12-22

Abstract

The invention provides a compound herbicide containing glufosinate-ammonium, which comprises effective components and auxiliary materials, wherein the effective components comprise 0.5-10 mass percent: 1, and cloflupirtine and isooctyl fluroxypyr. The compound herbicide disclosed by the invention has the beneficial effects that the interaction effect is formed between the clomazone and the fluroxypyr isooctyl acetate, wherein the price of the fluroxypyr isooctyl acetate is obviously lower than that of the clomazone, compared with the same-medicinal-component-dosage clomazone herbicide, the compound herbicide disclosed by the invention has the advantages that the application cost is reduced, the weed control effect is improved, and the drug resistance of weeds to the clomazone can be reduced. The invention optimizes the formulation of different dosage forms, ensures the drug effect of the preparation while using fewer auxiliary materials through auxiliary material selection and compounding of each component, and can further reduce the cost, thereby ensuring that the compound herbicide of the invention has higher market popularization value and economic benefit.

Description

Compound herbicide containing glufosinate-ammonium

Technical Field

The invention belongs to the field of herbicides, and particularly relates to a compound herbicide containing glufosinate-ammonium.

Background

The glufosinate-ammonium is a high-efficiency, low-toxicity and nonselective contact-killing type phosphoric acid herbicide. The glufosinate-ammonium is L-glufosinate-ammonium, and the weeding activity is twice as high as that of the racemic DL-glufosinate-ammonium mixture. The glufosinate-ammonium has very good water solubility, stable structure and convenient processing and mixing use. Under the large environment of pesticide decrement and synergy, the glufosinate-ammonium is a good substitute for the biocidal herbicide. However, the long-term single use of the glufosinate-ammonium can generate drug resistance and reduce the weed control effect, and the price of the glufosinate-ammonium is higher than that of the traditional biocidal herbicides such as glyphosate and the like at present, so that the market is limited.

The biological activities of different herbicides are different, the weed killing spectrum is different, and the synergistic effect can be achieved by compounding the herbicide. The compound use of the glufosinate-ammonium and other herbicides can possibly achieve better weeding effect while reducing the dosage of the glufosinate-ammonium, reduce the price of the herbicides while improving the weeding effect, ensure the safe growth of crops and reduce the environmental pollution, so that more compound herbicides containing the glufosinate-ammonium are necessary to be developed.

Disclosure of Invention

The invention aims to provide a compound herbicide containing glufosinate-ammonium.

In order to solve the technical problems, the invention adopts the following technical scheme:

the compound herbicide containing the glufosinate-ammonium comprises active ingredients and auxiliary materials, wherein the active ingredients comprise the glufosinate-ammonium and the fluroxypyr isooctyl ester, and the mass ratio of the glufosinate-ammonium to the fluroxypyr isooctyl ester is 0.5-10: 1, for example 0.5: 1. 1: 1. 2: 1. 3: 1. 4: 1. 5:1. 6: 1. 7: 1. 8: 1. 9: 1. 10:1. more preferably 1 to 5:1.

preferably, the active ingredients consist of glufosinate-ammonium and fluroxypyr-meptyl.

Preferably, the active ingredient comprises 15% -75% of the total mass of the compound herbicide, for example 15%, 20%, 25%, 30%, 235%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%.

Preferably, the auxiliary materials comprise 5% -40% of surfactant by weight of the total weight of the compound herbicide.

Further preferably, the surfactant is one or a combination of more than one of wetting agent, emulsifying agent and dispersing agent.

Still further preferably, the surfactant is one or more of fatty alcohol polyoxyethylene ether, alkylbenzene sulfonate, polycarboxylate, polyether ammonium sulfonate, phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt, sodium laureth sulfate, alkyl sulfate, and N, N-dimethyl sunflower amide.

Further preferably, the auxiliary material further comprises one or more of an antifreezing agent, a solvent, a filler, a disintegrating agent and a binder.

Still further preferably, the antifreeze is one or a combination of more of glycerol, propylene glycol, and ethylene glycol.

Still further preferably, the solvent is one or more of water, ethanol, methanol, N-dimethylformamide, dimethyl sulfoxide, cyclohexanone, methyl oleate, and vegetable oil.

Still further preferably, the filler is one or a combination of a plurality of diatomite, kaolin, bentonite, white carbon black and light calcium carbonate.

Still further preferably, the disintegrant is one or more of ammonium sulfate, urea, sodium sulfate, starch and its derivatives, cellulose, sodium bicarbonate, sodium lauryl sulfate, sodium alginate, 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.

According to some preferred embodiments, the formulation of the compound herbicide is an oil suspension comprising an active ingredient, a surfactant, a filler and an organic solvent, wherein the surfactant is at least two of fatty alcohol polyoxyethylene ether, alkylbenzene sulfonate, polycarboxylate and polyether ammonium sulfonate.

According to some preferred embodiments, the formulation of the compound herbicide is a suspoemulsion, which comprises an active ingredient, a surfactant, cyclohexanone and water, wherein the surfactant is at least two of fatty alcohol polyoxyethylene ether, alkylbenzene sulfonate, polycarboxylate, phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt and laureth sodium sulfate.

According to some preferred embodiments, the formulation of the compound herbicide is emulsifiable powder, which comprises an active ingredient, a surfactant and a filler, wherein the surfactant is at least two of polycarboxylate, alkyl sulfate and phenethyl phenol polyoxyethylene ether.

The emulsifiable powder is prepared by dissolving the effective components of the oil phase with the surface activity and the solvent, then adsorbing the effective components with solid phase wettable powder, and then shearing the obtained product at high speed to obtain a qualified emulsifiable powder preparation, wherein the emulsifiable powder has better efficacy than the conventional wettable powder because of finer particle size of the effective components and the existence of the solvent.

According to some embodiments, the formulation of the formulated herbicide is an oil suspension comprising, in mass percent:

according to other embodiments, the formulation of the compound herbicide is a suspoemulsion, which comprises the following components in percentage by mass:

according to still other embodiments, the dosage form of the formulated herbicide is an emulsifiable powder comprising, in mass percent:

35% -75% of active ingredients;

10% -25% of a surfactant;

5-15% of N, N-dimethylformamide;

10 to 40 percent of filler.

Preferably, when the formulation of the compound herbicide is an oil suspension, the surfactant is a combination of fatty alcohol-polyoxyethylene ether and alkylbenzene sulfonate, respectively.

Preferably, when the formulation of the compound herbicide is a suspoemulsion, the surfactant is a combination of fatty alcohol-polyoxyethylene ether, alkylbenzene sulfonate and polycarboxylate.

Preferably, when the formulation of the compound herbicide is emulsifiable powder, the surfactant is a combination of polycarboxylate, alkyl sulfate and fatty alcohol-polyoxyethylene ether.

According to some specific and preferred embodiments, the formulation of the formulated herbicide is an oil suspension comprising, in mass percent:

according to other specific and preferred embodiments, the formulation of the compound herbicide is a suspoemulsion comprising the following components in mass percent:

according to still other specific and preferred embodiments, the formulation of the formulated herbicide is an emulsifiable powder comprising, in mass percent:

the invention also provides application of the compound herbicide in preventing and controlling one or more of barnyard grass, green bristlegrass, crabgrass, purslane, goosegrass, common fleabane herb or common fleabane herb.

Preferably, the compound herbicide of the invention is used for preventing and controlling grape field additive weeds.

Due to the implementation of the technical scheme, compared with the prior art, the invention has the following advantages:

compared with the compound herbicide with the same or similar dosage of medicinal components, the compound herbicide has obviously improved control effects on barnyard grass, green bristlegrass, crabgrass, purslane, erigeron breviscapus and the like in the grape fields, and can reduce the dosage of the compound herbicide to reduce the drug resistance of weeds to the compound herbicide, wherein the price of the fluroxypyr isooctyl acetate is obviously lower than that of the compound herbicide, thereby improving the weed control effect while reducing the drug cost. Furthermore, the invention optimizes the formulation of different dosage forms, and the components of the herbicide are compounded by selecting auxiliary materials, so that the drug effect of the preparation is ensured while fewer auxiliary materials are used, the auxiliary materials are common and easy to obtain, and the cost can be further reduced, thereby the compounded herbicide of the invention has higher market popularization value and economic benefit.

Detailed Description

The present invention will be described in further detail with reference to specific examples. It should be understood that these examples are provided to illustrate the basic principles, main features and advantages of the present invention, and that the present invention is not limited by the following examples. The implementation conditions employed in the examples may be further adjusted according to specific requirements, and the implementation conditions not specified are generally those in routine experiments.

The glufosinate-ammonium TC (purity > 97%) was purchased from Qizhou green chemical company, inc.;

10% aqueous glufosinate (on frightened days) was purchased from Shandong Yisheng industries, inc.;

isooctyl fluroxypyr TC (purity > 97%) was purchased from Hubei De Ante chemical technology Co., ltd;

200g/L of fluroxypyr meptyl ester emulsifiable concentrate (pesticide registration number: PD 20081316) is purchased from Jiangxi Jiangnan green shore ecological technology Co., ltd;

fatty alcohol polyoxyethylene ether (AEO-9) was purchased from the sea Ann petrochemical plant in Jiangsu province;

alkylbenzene sulfonate (sodium dodecylbenzene sulfonate, rhodacal DS-10) was purchased from Shanghai, inc. of network technologies, inc.;

polycarboxylate (SD-816) was purchased from Shanghai as a macromolecular material Co., ltd;

polyether ammonium sulfonate (222) was purchased from Jiangsu Hao chemical Co., ltd;

alkyl sulfate (VT 859) was purchased from siebygaku chemical (shanghai) limited;

phenethyl phenol polyoxyethylene ether (601) was purchased from the company of katana chemical company, of Yixing, city;

the phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt (pesticide emulsion 600P) is purchased from Linyi national chemical industry Co., ltd;

sodium lauryl ether sulfate (KLY 663) was purchased from clarinet (shandong) biotechnology limited;

n, N-dimethyl-sunflower amide (CM) was purchased from Jiangsu Wannian pharmaceutical Co., ltd;

cyclohexanone is purchased from Shanghai Meilin Biochemical technologies Co., ltd;

methyl oleate was purchased from shandong chemical industry limited;

white carbon black (DL-620, 300 mesh gauge) was purchased from syn nan de lan chemical company, ltd;

kaolin (particle size: 2.34 μm) was purchased from Shanghai Valley grinding Co.

In the development process of the early-stage compound herbicide containing the glufosinate-ammonium, the effect of weeding can be better achieved by combining any herbicide with the glufosinate-ammonium, the weeding effect of the compound herbicide is related to the effective components, and the selection and the proportion of other components have more or less influence on the efficacy. Through a great deal of research and experimental verification, the inventor selects the combination of the fluroxypyr and the isooctyl fluroxypyr, and can improve the weed control effect while reducing the dosage of the glufosinate. The price of the current commercial crude drug of the smart glufosinate is about 11 ten thousand/ton, the price of the commercial crude drug of the fluroxypyr is about 7 ten thousand/ton, and the two can be used in a compound way, so that the cost of the crude drug is reduced and the weed control effect is improved. Further, the present application also provides for different dosage forms and preferred formulations for each dosage form, providing more options for the user.

Before developing different preparations, the influence of a compound composition of clomazone and fluroxypyr under room-temperature potting conditions on weed activity is studied by referring to a stem and leaf spray method of pesticide bioassay technology (published by Chen Chun, beijing agricultural university Press) and pesticide industry standards of the people's republic of China (pesticide indoor bioassay test criteria herbicide NY/T1155.3-2006, 1155.4-2006). The test target weeds were goosegrass, crabgrass, gooseberry and suaeda salsa. The indoor potting test results show that the composition of the glufosinate-ammonium and the fluroxypyr under different compounding proportions shows different degrees of additive or synergistic effects on the efficacy of the indoor potting, and no obvious antagonism exists. In the early room temperature potting test, the inventor also tries to compound acetochlor, metolachlor, glyphosate, dicamba, bispyribac-sodium and the like with the smart glufosinate, but the control effect is inferior to that of a composition of the smart glufosinate and the fluroxypyr.

Based on the results of the indoor potting test, the inventor of the application further performs a great deal of researches and experimental verification on auxiliary material selection and formulation of the formulation, so that more choices can be provided for users, and the following examples show some preferred formulations of different formulations and drug effect evaluation.

Examples 1-9 provide various formulations of the smart glufosinate-fluroxypyr isooctyl ester oil suspending agent, and specific components are shown in table 1, wherein "%" in table 1 is the mass percentage.

TABLE 1

The preparation method of the oil suspending agent comprises the following steps:

according to 1kg of the refined glufosinate-fluroxypyr isopropyl oil suspending agent, according to table 1, weighing each component, adding methyl oleate into a stirring device, adding each component into the methyl oleate, stirring at 180 revolutions per minute until the raw materials are wetted, and performing sand grinding by a sand mill to obtain the refined glufosinate-fluroxypyr isopropyl oil suspending agent.

The efficacy of the clomazone-fluroxypyr isooctyl oil suspension agent of examples 1-9 for controlling weeds in a field of grape is tested by referring to the GB/T17980.46-2000 pesticide field efficacy test criteria.

The test site is Jiangsu province Zhang Jianggang Dazhen, and the test field is a 5-year vineyard. Test Tian Deshi was flat, sandy loam. The pesticide is applied in the afternoon in 6 months of 2021, the grapes are in the flowering period, the row spacing of the grape fields is 1.5m, the weeds in the grape fields comprise annual weeds (goosegrass, crabgrass and calfskin) and perennial weeds (erigeron breviscapus are mainly), the weeds are in the 3-4 leaf growth period, and the plant height is different from 15 cm to 30 cm. The weather of the day of the drug application is cloudy, the highest temperature is 25 ℃, the lowest temperature is 16 ℃, and no wind exists. And 3 days after the medicine, no rainfall weather exists.

Test cell division: and selecting a district with weed coverage of 80% or more per 66 square meters of district area.

The application method comprises the following steps: the preparation is weighed according to the dosage of each mu of preparation in table 2, 30L of water is added according to the dosage of each mu of preparation for dilution, and after dilution, directional spraying is carried out on weeds among grape rows by adopting a backpack electric sprayer, so that the liquid medicine is prevented from being sprayed on the grapes as much as possible. The dosage of the treatment agent for each test cell is shown in Table 2, three replicates are set for each formulation, the statistical average is calculated, and the cells treated with different agents are arranged in a completely random block. Two groups of non-application test cells were set as blank controls, 10% of glufosinate-ammonium aqueous solution and 200g/L of fluroxypyr isooctyl ester emulsifiable concentrate were used as controls, the dosage of the control agents is shown in Table 2, and three repeated cells were set for each control.

Investigation method and drug efficacy evaluation method: the control effect of each plot was investigated by 14d and 30d after the application of the composition, and the 3-point sampling method was adopted, wherein each point was selected to be 0.5 square meter, the types and the plant numbers of weeds were recorded, the weed plant control effect was calculated, and the statistics of the annual weeds such as goosegrass, crabgrass, goosefoot and perennial weeds such as eries were counted in table 2. While the effect on grape growth was visually observed.

TABLE 2

Table 2 shows that the effect of the clomazone-fluroxypyr isooctyl ester oil suspension agent on preventing weeds in grape fields is higher than that of the clomazone aqueous agent and the fluroxypyr isooctyl ester emulsifiable concentrate under the condition of basically the same effective component dosage. The weed control effect of the refined glufosinate-fluroxypyr isooctyl oil suspending agent composed of refined glufosinate, fluroxypyr, fatty alcohol polyoxyethylene ether, alkylbenzene sulfonate, bentonite and methyl oleate is better.

Examples 10 to 18 provide various formulations of the suspension emulsion of the glufosinate-fluroxypyr and the isooctyl, the specific components are shown in Table 3, and "%" in Table 3 is the mass percent.

TABLE 3 Table 3

The preparation method of the suspension emulsion comprises the following steps:

according to 1kg of the smart glufosinate-fluroxypyr-meptyl suspending agent, each component is weighed according to the table 3, cyclohexanone is added into a stirring device, then the other components are added into the cyclohexanone, the mixture is stirred at 180 revolutions per minute until the mixture is uniform, and the mixture is sanded by a sand mill to prepare the smart glufosinate-fluroxypyr-meptyl suspending agent.

The pesticide effect of the clomazone fluroxypyr suspending agent of examples 10 to 18 for controlling weeds in the field of grapes is tested by referring to the GB/T17980.46-2000 pesticide field efficacy test criteria. Test methods and weed plant control calculations reference oil suspensions, dosage of the agents and weed plant control results are shown in table 4.

TABLE 4 Table 4

Table 4 shows that the prevention effect of the suspension agent of the clomazone and the fluroxypyr on weeds is higher than that of the emulsion of the clomazone and the fluroxypyr under the condition of similar effective component amounts. Wherein, the suspension of the clomazone fluoxymate and the cloflupyrxymate, which consists of the clomazone, the fatty alcohol polyoxyethylene ether, the alkylbenzene sulfonate, the polycarboxylate, the cyclohexanone and the water, has better weeding effect.

Examples 19-28 provide various formulations of the arginate-fluroxypyr-meptyl emulsifiable powder, the specific components are shown in Table 5, and "%" in Table 5 is the mass percent.

TABLE 5

The preparation method of the emulsifiable powder comprises the following steps:

according to 1kg of the emulsifiable powder of the clomazone-fluroxypyr, according to the table 5, weighing each component, stirring the clomazone-fluroxypyr and diatomite uniformly, carrying out superfine grinding (98% screening by a 325-mesh sieve) by a jet mill, mixing and dissolving the clomazone-fluroxypyr, N-dimethyl-sunflower amide and fatty alcohol polyoxyethylene ether uniformly, then slowly adding the mixture into the clomazone powder, and stirring uniformly at a speed of 100-150 rpm to obtain the emulsifiable powder of the clomazone-fluroxypyr.

The pesticide effect of the clomazone fluroxypyr emulsifiable powder of examples 19 to 28 for controlling weeds in the field of grapes was tested by referring to the GB/T17980.46-2000 pesticide field efficacy test criteria. Test methods and weed plant control calculations reference oil suspensions, dosage of the agents and weed plant control results are shown in table 6.

TABLE 6

Table 6 shows that the emulsifiable powder of the clomazone-fluroxypyr has higher prevention effect on weeds than the clomazone-fluroxypyr emulsifiable concentrate under the condition of similar effective component amounts. Wherein, the weeding effect of the emulsifiable powder of the glufosinate-fluroxypyr is better, wherein the emulsifiable powder comprises the glufosinate-fluroxypyr, the polycarboxylate, the alkyl sulfate, the fatty alcohol-polyoxyethylene ether, the N, N-dimethyl-sunflower amide, the white carbon black and the kaolin.

The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement it accordingly, and are not intended to limit the scope of the present invention, but all equivalent changes or modifications according to the spirit of the present invention should be included in the scope of the present invention.

Claims

1. The compound herbicide containing the glufosinate-ammonium comprises active ingredients and auxiliary materials, and is characterized in that: the active ingredients comprise the smart glufosinate and the fluroxypyr isooctyl ester, and the mass ratio of the smart glufosinate to the fluroxypyr isooctyl ester is 0.5-10: 1.

2. the formulated herbicide of claim 1, wherein: the active ingredients consist of glufosinate-ammonium and fluroxypyr-meptyl;

and/or the effective components account for 15-75% of the total mass of the compound herbicide.

3. The formulated herbicide of claim 1, wherein: the auxiliary materials comprise 5% -40% of surfactant in total weight of the compound herbicide.

4. The formulated herbicide of claim 1, wherein: the surfactant is one or a combination of more of fatty alcohol polyoxyethylene ether, alkylbenzene sulfonate, polycarboxylate, polyether ammonium sulfonate, phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt, sodium laureth sulfate and alkyl sulfate.

5. The formulated herbicide of claim 4, wherein: the auxiliary materials also comprise one or a combination of more of an antifreezing agent, a solvent, a filler, a disintegrating agent and a binder;

the antifreezing agent is one or a combination of more of glycerol, propylene glycol and ethylene glycol;

the solvent is one or a combination of more of water, ethanol, methanol, N-dimethylformamide, N-dimethyl-sunflower-amide, dimethyl sulfoxide, cyclohexanone, methyl oleate and vegetable oil;

the filler is one or a combination of a plurality of diatomite, kaolin, bentonite, white carbon black and light calcium carbonate;

the disintegrating agent is one or a combination of more of ammonium sulfate, urea, sodium sulfate, starch and derivatives thereof, cellulose, sodium bicarbonate, sodium lauryl sulfate, sodium alginate and sodium chloride;

6. The formulated herbicide of claim 4, wherein: the formulation of the compound herbicide is an oil suspending agent, which comprises an effective component, a surfactant, a filler and an organic solvent, wherein the surfactant is at least two of fatty alcohol polyoxyethylene ether, alkylbenzene sulfonate, polycarboxylate and polyether ammonium sulfonate;

or the formulation of the compound herbicide is a suspension emulsion, and comprises an effective component, a surfactant, cyclohexanone and water, wherein the surfactant is at least two of fatty alcohol polyoxyethylene ether, alkylbenzene sulfonate, polycarboxylate, phenethyl phenol polyoxyethylene ether phosphate triethanolamine salt and lauryl alcohol ether sodium sulfate;

or the dosage form of the compound herbicide is emulsifiable powder, and comprises an effective component, a surfactant and a filler, wherein the surfactant is at least two of polycarboxylate, alkyl sulfate and phenethyl phenol polyoxyethylene ether.

7. The formulated herbicide of claim 1, wherein: the formulation of the compound herbicide is an oil suspending agent, and comprises the following components in percentage by mass:

or, the formulation of the compound herbicide is a suspoemulsion, and comprises the following components in percentage by mass:

or the dosage form of the compound herbicide is emulsifiable powder, and comprises the following components in percentage by mass:

35% -75% of active ingredients;

10% -25% of a surfactant;

5-15% of N, N-dimethylformamide;

10 to 40 percent of filler.

8. The formulated herbicide of claim 1, wherein: when the formulation of the compound herbicide is an oil suspending agent, the surfactant is respectively a composition of fatty alcohol polyoxyethylene ether and alkylbenzene sulfonate;

or when the formulation of the compound herbicide is a suspoemulsion, the surfactant is a composition of fatty alcohol polyoxyethylene ether, alkylbenzene sulfonate and polycarboxylate;

or when the formulation of the compound herbicide is emulsifiable powder, the surfactant is a composition of polycarboxylate, alkyl sulfate and fatty alcohol polyoxyethylene ether.

9. The formulated herbicide of claim 8, wherein: the formulation of the compound herbicide is an oil suspending agent, and comprises the following components in percentage by mass:

10. use of a formulated herbicide as claimed in any one of claims 1 to 9 for controlling one or more of barnyard grass, green bristlegrass, crabgrass, purslane and horsetail.