Weeding composition containing sethoxydim and clopyralid as well as preparation method and application of weeding composition

Abstract

The invention relates to the technical field of pesticides, and discloses a weeding composition containing sethoxydim and clopyralid as well as a preparation method and application of the weeding composition. The composition comprises sethoxydim and clopyralid, and the mass ratio of sethoxydim to clopyralid is (3-8): (9-27). The weeding composition disclosed by the invention can be used for effectively preventing and removing annual weeds in a foxtail millet field, and in addition, the weeding composition is safe and non-toxic to foxtail millet.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of pesticides, and relates to a herbicidal composition containing sethoxydim and clopyralid as well as a preparation method and application thereof. BACKGROUND

[0002] Sethoxydim is a cyclohexenone selective systemic herbicide, ACCase inhibitor, usually used for stem-leaf treatment to control grass weeds. It is absorbed by the stems and leaves of weeds and conducted to the apical and intercalary meristems, thereby causing cell division and destruction. Sethoxydim is generally suitable for soybean, cotton, rapeseed, peanut, sugar beet, flax, broadleaf vegetable, potato and orchard, etc.

[0003] Clopyralid is a synthetic hormone systemic herbicide, mainly absorbed by the stems and leaves of plants, conducted through the phloem and xylem, accumulated in the growth point, causing the plant to produce excess ribonucleic acid, promoting the excessive differentiation of meristems, abnormal growth of roots, stems and leaves, excessive consumption of nutrients, and blocked vascular transport function, thereby causing the death of weeds. Clopyralid can also be conducted to the roots through the xylem, completely killing deep-rooted weeds. In sensitive plants, clopyralid can induce typical hormone responses, such as stem twisting and curling, cup-shaped leaves, root thickening, poor root hair development, stem brittleness, easy breakage, and excessive proliferation of root meristems, stem and root warts, and inhibition of root and aboveground growth. Clopyralid is generally suitable for controlling broadleaf weeds in rapeseed, wheat, corn, cruciferous vegetables, sugar beet, flax, strawberry, and grass lawn.

[0004] Millet has important position and development potential in dry farming due to its drought and barren tolerance, but weed damage is serious in its production, and manual weeding has high labor intensity, high cost and low efficiency. Chemical weeding is one of the main means of controlling weeds in agriculture. According to the existing reports and actual test screening verification, millet is extremely sensitive to many chemical herbicide varieties. At present, there are few registered herbicides for use on millet in China, and the varieties are single. Actual use often has poor weeding effect, or easily causes serious millet phytotoxicity and even seedling death. Weed control has been one of the main obstacles to the industrialized production of millet.

[0005] Compounding pesticide active ingredients with different mechanisms of action is an effective way to develop and research new pesticides. Based on the purpose of comprehensive control of millet field weeds and market demand, there is an urgent need for a safe and efficient herbicidal composition. SUMMARY

[0006] The applicant finds through a large number of experiments that the aryloxyacetic acid and the dichloropyridine acid have inhibitory effects on annual weeds such as dogtail grass and alternanthera philoxeroides. Further research finds that the herbicidal composition of the present application is applied to millet fields, and the stems and leaves are sprayed at the 3-5 leaf stage of the millet, which can effectively prevent and control annual weeds of the gramineous weeds and broadleaf weeds, and has no effect on the growth of the millet, which indicates that the composition or the herbicidal preparation of the present application has high safety. There is no report on the aryloxyacetic acid and the dichloropyridine acid being used for removing weeds in millet fields.

[0007] On the basis of further research, the present application is completed.

[0008] The present application provides a herbicidal composition containing aryloxyacetic acid and dichloropyridine acid, which comprises aryloxyacetic acid and dichloropyridine acid, and the mass ratio of the aryloxyacetic acid and the dichloropyridine acid is 3-8:9-27.

[0009] Preferably, the mass ratio of the aryloxyacetic acid and the dichloropyridine acid is 5:18.

[0010] The present application also provides a herbicidal preparation comprising the herbicidal composition described above.

[0011] Preferably, the mass percentage of the herbicidal composition is 10-75wt% based on the total mass of the herbicidal preparation.

[0012] Preferably, the dosage form of the herbicidal preparation is dispersible oil suspension.

[0013] More preferably, the preparation method of the dispersible oil suspension is that the herbicidal composition, the emulsifier, the dispersant and the viscosity regulator are mixed and sand ground. The specific steps are as follows: the metered aryloxyacetic acid, dichloropyridine acid, emulsifier, dispersant, viscosity regulator and methyl oleate are added into a jacketed shear kettle for shearing, cooling water is passed during shearing, the shearing temperature is controlled to be less than 30 DEG C, sand grinding is performed after uniform dispersion, the sand grinding temperature is controlled to be less than 20 DEG C throughout the sand grinding process, and sand grinding is performed until the particle size D 90 <5um, and then the sample is detected and qualified before being filled.

[0014] The present application also provides the application of the herbicidal composition described above or the herbicidal preparation described above in removing weeds or preparing a product for removing weeds.

[0015] Preferably, the application comprises removing annual weeds in millet fields.

[0016] More preferably, the annual weeds are selected from one or both of dogtail grass and alternanthera philoxeroides.

[0017] More preferably, the millet in the millet field is at the 3-5 leaf stage.

[0018] Preferably, the herbicidal composition or the herbicidal formulation is used in the form of foliage spraying.

[0019] Compared with the prior art, the present application has the following beneficial effects: 1. The herbicidal composition or the herbicidal formulation of the present application is obtained by compounding the active ingredients of fenclorim and clopyralid, has obvious synergistic effect, and can improve the control effect on annual weeds, especially can significantly improve the control effect on Digitaria sanguinalis and Acalypha australis.

[0020] The herbicidal composition or the herbicidal formulation of the present application can delay the generation of weed resistance.

[0021] After the herbicidal composition or the herbicidal formulation of the present application is used by spraying in millet fields, the millet grows normally and is safe to the millet. DETAILED DESCRIPTION

[0022] The present application will be further described below in conjunction with specific examples, but the present application is not limited to these specific examples. Those skilled in the art should realize that the present application encompasses all alternatives, improvements, equivalents within the scope of the claims.

[0023] Example 1: Indoor activity test of fenclorim and clopyralid combination Test purpose: Through indoor bioassay test, the indoor control effect of fenclorim and clopyralid combination on Digitaria sanguinalis and Acalypha australis is determined, the joint action is evaluated, and the herbicidal activity of the combination and single agent is further compared, so as to better illustrate the present application.

[0024] Test target: Digitaria sanguinalis and Acalypha australis seeds, both of which are collected from traditional millet planting areas and stored indoors for standby use.

[0025] Test method: Fine soil is loaded into a plastic pot with holes, and the pot bottom is used for drip irrigation to make the soil completely wet. After the Digitaria sanguinalis and Acalypha australis seeds are soaked for 12 hours, they are evenly sowed on the soil surface, 30 seeds per pot, and then covered with about 0.5 cm thick fine soil. The pot bottom is used for drip irrigation to make the soil wet. According to the Pesticide Indoor Bioassay Test Guidelines, 3-4 leaf stage test weeds with uniform growth are selected for foliage spraying treatment, and the spraying amount is 40 mL / m 2 , and the weeds are sprayed once. After 14 days, the fresh weight of the aboveground parts of Digitaria sanguinalis and Acalypha australis is investigated, and the fresh weight inhibition rate (i.e. control effect) is calculated.

[0026] Joint action evaluation: the joint action mode of two herbicides is evaluated by Gowing method (NY / T 1155.7-2006), and the calculation formula is: E0=X+Y-XY / 100. In the formula, X represents the measured control effect of herbicide A when the dosage is P; Y represents the measured control effect of herbicide B when the dosage is Q; E0 is the theoretical control effect of herbicide A when the dosage is P + the theoretical control effect of herbicide B when the dosage is Q; E is the measured control effect after mixing herbicide A and herbicide B according to the above proportion; in this application, A is fenclorim, and B is clopyralid.

[0027] According to Gowing method, E-E0>10% is synergistic effect; E-E0<-10% is antagonistic effect; E-E0 value between ±10% is additive effect.

[0028] Table 1: indoor toxicity of fenclorim, clopyralid single agent and its compound for controlling Digitaria sanguinalis and acacia constricta According to the indoor toxicity determination test results in Table 1, when the mass ratio of fenclorim and clopyralid is 56.25-150:168.75-506.25, i.e. 3-8:9-27, each treatment produces synergistic effect or positive additive effect for controlling Digitaria sanguinalis and acacia constricta. In particular, when the mass ratio of fenclorim and clopyralid is 93.75:337.5 (i.e. 5:18), very significant synergistic effect is produced for controlling Digitaria sanguinalis and acacia constricta. It can be seen that the herbicidal composition formed by the compound of fenclorim and clopyralid has better herbicidal effect.

[0029] The following specifically lists examples of herbicidal formulations for further proving the advantages of the present application, but the present application is not limited thereto. Unless otherwise specified, the percentages in the following examples are mass percentages.

[0030] Example 2: herbicidal formulation In this example, herbicidal formulations containing various different effective amount compositions are prepared and obtained. They include the following: Herbicidal formulation 1: 23% fenclorim.clopyralid (5:18) dispersible oil suspension 23% fenclorim.clopyralid dispersible oil suspension: composed of the following mass percentages of components, fenclorim 5 wt %, clopyralid 18 wt %, calcium dodecylbenzenesulfonate 7.5 wt %, triphenyl ethenyl phenol polyoxyethylene ether 10 wt %, EO-PO block polyoxyethylene ether 2 wt %, organic bentonite 1 wt %, and methyl oleate.

[0031] The mixed material is subjected to high-speed shearing until the material is uniformly dispersed, cooling water is passed during shearing, the shearing temperature is controlled to be <30°C, the sand milling temperature is controlled to be <20°C throughout the sand milling process, and sand milling is performed until the particle size D90 <5 μm, in the preparation kettle, sampling detection qualified after filling.

[0032] Herbicidal formulation 2: 17% clodinafop-propargyl + clopyralid (5:12) dispersible oil suspension 17% clodinafop-propargyl + clopyralid dispersible oil suspension: composed of the following mass percentage of components, clodinafop-propargyl 5 wt %, clopyralid 12 wt %, calcium dodecyl benzene sulfonate 8 wt %, triphenyl ethenyl phenol polyoxyethylene ether 10 wt %, EO-PO block polyoxyethylene ether 2.5 wt %, organic bentonite 1 wt %, methyl oleate.

[0033] The mixed material is subjected to high-speed shearing until the material is uniformly dispersed, cooling water is passed during shearing, the shearing temperature is controlled to be <30°C, the sanding temperature is controlled to be <20°C throughout the sanding process, and the sanding is performed until the particle size D 90 <5 μm, in the preparation kettle, sampling detection qualified after filling.

[0034] Herbicidal formulation 3: 32% clodinafop-propargyl + clopyralid (5:27) dispersible oil suspension 32% clodinafop-propargyl + clopyralid dispersible oil suspension: composed of the following mass percentage of components, clodinafop-propargyl 5 wt %, clopyralid 27 wt %, calcium dodecyl benzene sulfonate 9 wt %, triphenyl ethenyl phenol polyoxyethylene ether 8 wt %, EO-PO block polyoxyethylene ether 2.5 wt %, organic bentonite 1 wt %, methyl oleate.

[0035] The mixed material is subjected to high-speed shearing until the material is uniformly dispersed, cooling water is passed during shearing, the shearing temperature is controlled to be <30°C, the sanding temperature is controlled to be <20°C throughout the sanding process, and the sanding is performed until the particle size D 90 <5 μm, in the preparation kettle, sampling detection qualified after filling.

[0036] Herbicidal formulation 4: 21% clodinafop-propargyl + clopyralid (3:18) dispersible oil suspension 21% clodinafop-propargyl + clopyralid dispersible oil suspension: composed of the following mass percentage of components, clodinafop-propargyl 3 wt %, clopyralid 18 wt %, calcium dodecyl benzene sulfonate 7.5 wt %, triphenyl ethenyl phenol polyoxyethylene ether 11 wt %, EO-PO block polyoxyethylene ether 2 wt %, organic bentonite 1 wt %, methyl oleate.

[0037] The mixed material is subjected to high-speed shearing until the material is uniformly dispersed, cooling water is passed during shearing, the shearing temperature is controlled to be <30°C, the sanding temperature is controlled to be <20°C throughout the sanding process, and the sanding is performed until the particle size D 90<5 μm, in the preparation kettle, sampling detection qualified after filling.

[0038] Herbicidal formulation 5: 27% fluazifop-butyl. clopyralid (3:24) dispersible oil suspension 27% fluazifop-butyl. clopyralid dispersible oil suspension: composed of the following mass percentage of components, fluazifop-butyl 3 wt %, clopyralid 24 wt %, calcium dodecyl benzene sulfonate 8 wt %, triphenyl styryl phenol polyoxyethylene ether 9 wt %, EO-PO block polyoxyethylene ether 2 wt %, organic bentonite 1 wt %, methyl oleate.

[0039] The mixed material is subjected to high-speed shearing until the material is uniformly dispersed, cooling water is passed during shearing, the shearing temperature is controlled to be <30°C, the sanding temperature is controlled to be <20°C throughout the sanding process, and sanding is performed until the particle size D90 is <5 μm. 90 <5 μm, in the preparation kettle, sampling detection qualified after filling.

[0040] Herbicidal formulation 6: 26% fluazifop-butyl. clopyralid (8:18) dispersible oil suspension 26% fluazifop-butyl. clopyralid dispersible oil suspension: composed of the following mass percentage of components, fluazifop-butyl 8 wt %, clopyralid 18 wt %, calcium dodecyl benzene sulfonate 6 wt %, triphenyl styryl phenol polyoxyethylene ether 12 wt %, EO-PO block polyoxyethylene ether 2.5 wt %, organic bentonite 1 wt %, methyl oleate.

[0041] The mixed material is subjected to high-speed shearing until the material is uniformly dispersed, cooling water is passed during shearing, the shearing temperature is controlled to be <30°C, the sanding temperature is controlled to be <20°C throughout the sanding process, and sanding is performed until the particle size D90 is <5 μm.

[0042] Herbicidal formulation 7: 17% fluazifop-butyl. clopyralid (8:9) dispersible oil suspension 17% fluazifop-butyl. clopyralid dispersible oil suspension: composed of the following mass percentage of components, fluazifop-butyl 8 wt %, clopyralid 9 wt %, calcium dodecyl benzene sulfonate 5 wt %, triphenyl styryl phenol polyoxyethylene ether 11 wt %, EO-PO block polyoxyethylene ether 1.5 wt %, organic bentonite 1 wt %, methyl oleate.

[0043] The mixed material is subjected to high-speed shearing until the material is uniformly dispersed, cooling water is passed during shearing, the shearing temperature is controlled to be <30°C, the sanding temperature is controlled to be <20°C throughout the sanding process, and sanding is performed until the particle size D 90 <5 μm, in the preparation kettle, sampling detection qualified after filling.

[0044] Example 3 The indoor toxicity of the herbicidal preparation to millet and the selectivity between millet and dogtail grass Purpose of the test: millet and dogtail grass belong to the same genus of grasses, and their genes are highly similar. In order to better illustrate the herbicidal effect of the present application and the rationality of its use in millet fields, further, the stems and leaves of millet seedlings and dogtail grass of different varieties were treated with cloquintocet and clopyralid, respectively, to evaluate the safety of the test agents to millet and the selectivity of the test agents to millet and dogtail grass, so as to better illustrate the popularization value of the present application in millet fields.

[0045] Test targets: Shuxianghuang millet (yellow millet variety) and Hongxiu 38 (red millet variety), both of which are high-yield, disease-resistant and insect-resistant varieties available on the market. Dogtail grass seeds were collected in the field and stored in the laboratory for use.

[0046] Test method: Fine soil was loaded into plastic pots with holes, and the pots were watered from the bottom to make the soil completely wet. Millet and dogtail grass were pre-soaked to germinate and break the hull, and then evenly sowed on the soil surface, covered with 0.5 cm thick fine soil, and watered from the bottom to make the soil wet. The pots were placed in a greenhouse for cultivation and outdoor seedling training. Before application, the seedlings were thinned to retain 4-5 leaf age millet seedlings and dogtail grass seedlings with uniform growth vigor, 15 seedlings per pot, for treatment. According to the "Guidelines for Pesticide Indoor Biological Test", the stems and leaves were treated by spraying, the amount of spray was 40 mL / m 2 , and the drug was applied once.

[0047] Investigation method: 14 days after treatment, the absolute value method was used, the survival plants were cut off along the soil surface with a blade, and the fresh weight was measured and calculated for fresh weight control effect.

[0048] Fresh weight control effect = (control fresh weight - treatment fresh weight) / control fresh weight * 100.

[0049] The ED 10 values of the test agents to millet and the ED 90 values to dogtail grass were calculated by DPS software analysis, and the selectivity index of the test agents to different varieties of millet and dogtail grass under the test conditions was calculated.

[0050] Selectivity index = ED 10 value to millet / ED 90 value to weeds Table 2: Toxicity of the herbicidal preparation to millet and selectivity between millet and dogtail grass According to Table 2, the results of the toxicity of the herbicidal preparation to millet and the selectivity between millet and dogtail grass showed that the test agents had ED 90The value was 312.80 gai / ha, while the ED value for the tested millet varieties Shuxiang Huanggu and Hongxiu 38 was lower. 10 The values ​​were 1004.89 gai / ha and 911.92 gai / ha, respectively, with corresponding selectivity indices of 3.21 and 2.92, both significantly greater than 2. This indicates the safety of the herbicide (i.e., 23% tebuconazole·dichloropyridine OD) on millet and its effectiveness in controlling foxtail grass in millet fields, fully demonstrating that the herbicide combination or herbicide of this invention has excellent application value in controlling annual weeds in millet fields.

[0051] Example 4: Field efficacy test of different herbicides for controlling weeds in millet fields Test reagents: Herbicide Formulation Example 1: 23% clopyralid·dichloropyridine (5:18) OD: Herbicide formulation 2: 17% clopyralid.dichloropyridine (5:12) OD; Herbicide formulation 3: 32% clopyralid.dichloropyridine (5:27) OD; Herbicide formulation 4: 21% clopyralid.dichloropyridine (3:18) OD Herbicide formulation 5:27% clopyralid.dichloropyridine (3:24) OD; Herbicide formulation 6:26% clopyralid.dichloropyridine (8:18) OD; Herbicide formulation 7:17% clopyralid.dichloropyridine (8:9) OD; Control 1: 12.5% ​​tebufenozide EC (Zhongnong Lihua) Control 2: 75% dichloropyridine SG (Zhejiang Tianfeng); CK: Blank control Test location: Weixian County, Hebei Province The millet variety used in the experiment was Jigu 25. To ensure the uniformity of the target area for the herbicide application, foxtail grass and amaranth seeds were sown at the same time as the millet. Before application, the millet seedlings were observed to be at the 3-5 leaf stage, with a high proportion of seedlings at the 4-5 leaf stage. Barnyard grass, crabgrass, foxtail grass, and broadleaf weeds such as amaranth, reverse branch amaranth, and lambsquarters were all present in the field.

[0052] Each treatment was replicated four times, with each treatment plot measuring 10 m². 2 The mixture was arranged in a randomized block design. Each pesticide was diluted with 30 kg of water per acre at the recommended dosage and sprayed evenly.

[0053] Experimental survey method: Four points were randomly selected from each treatment plot, and each point was surveyed for 0.25m. 2The growth of millet and phytotoxicity symptoms in each treatment plot were observed after the treatment, the fresh weight of gramineous weeds and broadleaf weeds in each treatment plot was investigated 14 days after the treatment, and the fresh weight inhibition rate (control effect) was calculated. The test results are shown in Table 3.

[0054] Table 3: Weed control effect in millet field 14 days after application As can be seen from Table 3, the herbicidal formulations 1-7 have good control effects on annual gramineous weeds and broadleaf weeds in millet fields. Compared with the control herbicides 12.5% fluazifop-butyl EC (i.e. control 1) and 75% clopyralid SG (i.e. control 2), the herbicidal formulations of the present application have significantly improved individual control effect and comprehensive control effect on gramineous weeds and broadleaf weeds. In particular, the herbicidal formulation example 1 has a control effect on gramineous weeds and broadleaf weeds of more than 90%, and does not affect the normal growth of millet, and is safe to millet.

[0055] Although the present application has been described in detail with general description and specific examples above, some modifications or improvements can be made on the basis of the present application, which is obvious to those skilled in the art. Therefore, these modifications or improvements made on the basis of not deviating from the spirit of the present application, all belong to the scope of the present application claimed.

Claims

1. A herbicidal composition comprising cloquintocet and clopyralid, characterized in that, The fenclorim and the clopyralid are in a mass ratio of 3-8:9-27.

2. The herbicidal composition according to claim 1, characterized by The mass ratio of the fenclorim and the clopyralid is 5:

18.

3. A herbicidal preparation, characterized by comprising The herbicidal composition according to claims 1-2.

4. The herbicidal preparation according to claim 3, characterized in that The mass percentage of the composition is 10-75wt% based on the total mass of the herbicidal formulation.

5. The preparation according to claim 3 or 4, characterized in that, The dosage form of the herbicidal formulation is dispersible oil suspension.

6. The use of the composition according to claim 1 or the herbicidal formulation according to claim 3 in removing weeds or preparing a product for removing weeds.

7. Use according to claim 6, wherein The use includes removing weeds in a millet field.

8. Use according to claim 7, characterized in that, The weeds are annual weeds; and / or, the millet is at a 3-5 leaf stage; and / or, the herbicidal composition or herbicidal formulation is used in a foliar spray.

9. Use according to claim 8, characterized in that, The annual weeds are selected from one or both of crabgrass and acacia.

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