HERBICIDAL COMPOSITION, PREPARATION AND APPLICATION THEREOF

Abstract

The invention relates to the technical field of pesticides, in particular to a herbicidal composition, preparation and application thereof. The herbicidal composition comprises a component A and a component B, wherein, the component A is benzylazole, and the component B is at least one of acetochlor, butachlor, metolachlo, dimethylphenoxychlor, mesotrione, nicosulfuron, atrazine, terbuthylazine, metribuzin, S-metolachlor and dimethylphenoxychlor. The weight ratio of the component A to the component B is 1: (1-80).

Claims

1. A herbicidal composition, wherein the composition comprises a component A and a component B, wherein, the component A is benzylazole, and the component B is at least one of acetochlor, butachlor, metolachlo, dimethylphenoxychlor, mesotrione, nicosulfuron, atrazine, terbuthylazine, metribuzin, S-metolachlor and dimethylphenoxychlor; the weight ratio of the component A to the component B is 1: (1-80).

2. A herbicidal composition preparation, comprising the herbicidal composition of claim 1 and excipients acceptable in pesticide science.

3. The herbicidal composition preparation of claim 2, wherein the dosage form of the herbicidal composition preparation is one of emulsion, water emulsion, microemulsion, dispersible oil suspension, suspension emulsion, microcapsule suspension-water emulsion, wettable powder and water dispersible granule.

4. The herbicidal composition preparation of claim 2, wherein the herbicidal composition accounts for 1 to 90% of the weight of the herbicidal composition preparation.

5. The herbicidal composition preparation of claim 2, wherein the dosage form of the herbicidal composition preparation is water emulsion; the excipients acceptable in pesticide science comprise at least one of solvent, emulsifier, thickener, antifreeze agent, defoaming agent, density regulator and pH regulator.

6. The herbicidal composition preparation of claim 5, wherein the emulsifier is at least one of alkyl phenol polyoxyethylene ether, phenylethyl phenol polyoxyethylene polyoxypropylene ether, polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monopalmitate, polyoxyethylene sorbitan monostearate, sorbitan monooleate, sorbitan laurate, sorbitan monopalmitate, sorbitan stearate, castor oil polyoxyethylene ether, alkylbenzene sulfonate, alkyl naphthalene sulfonate and alkyl sulfonate.

7. The herbicidal composition preparation of claim 6, wherein the emulsifier is the combination of castor oil polyoxyethylene ether, sorbitan monopalmitate and sodium dodecylbenzene sulfonate at the weight ratio of (10-20): (1-5): 1.

8. The herbicidal composition preparation of claim 5, wherein the solvent is the combination of organic solvent and water, and the weight ratio of the organic solvent to the emulsifier is (2-5): 1.

9. The herbicidal composition preparation of claim 8, wherein the organic solvent is at least one of hydrocarbon solvent, ketone solvent, ester solvent, alcohol solvent and aromatic solvent.

10. The application of the herbicidal composition preparation of claim 5, wherein it is applied to the pre-seedling soil treatment of dry crops.

Description

DETAILED DESCRIPTION OF EMBODIMENTS

Embodiment 1

[0057] Embodiment 1 provides a water emulsion of herbicial composition, which is prepared by the raw materials comprising the following components by weight percentage: herbicidal composition 51%, emulsifier 4%, thickener 2%, antifreeze agent 1%, organic solvent 12% and water (the residual percentage).

[0058] The herbicidal composition is a combination of benzylazole and acetochlor with a weight ratio of 1:50; the emulsifier is a combination of castor oil polyoxyethylene ether, sorbitol monopalmitate and sodium dodecylbenzene sulfonate with a weight ratio of 16:3:1; the castor oil polyoxyethylene ether is purchased from Jiahua Chemical Co., Ltd. with the model of EL-30; the sorbitol monopalmitate is purchased from Jiangsu Hai'an Petrochemical Plant with the model of S-40; the sodium dodecylbenzene sulfonate is purchased from Langfang Pengcai Fine Chemical Co., Ltd.; the thickener is polyvinyl alcohol; the antifreeze agent is glycerol; the organic solvent is 150 #solvent oil; and the water is deionized water.

[0059] The preparation method of the water emulsion is as follows:

[0060] (1) Dissolve the herbicidal composition in an organic solvent, add an emulsifier and stir evenly to obtain an oil phase;

[0061] (2) Mix a thickener and an antifreeze agent with water to obtain a water phase;

[0062] (3) Slowly add the oil phase into the water phase under the condition of high-speed shear, and continue to shear for 40 min to obtain the water emulsion.

Embodiment 2

[0063] Embodiment 2 provides a water emulsion of herbicial composition, which is prepared by the raw materials comprising the following components by weight percentage: herbicidal composition 30%, emulsifier 3%, thickener 1%, antifreeze agent 0.5%, organic solvent 15% and water (the residual percentage);

[0064] The herbicidal composition is a combination of benzylazole and S-metolachlor metolachlor with a weight ratio of 1:50; the emulsifier is a combination of castor oil polyoxyethylene ether, sorbitol monopalmitate and sodium dodecylbenzene sulfonate with a weight ratio of 10:1:1; the castor oil polyoxyethylene ether is purchased from Jiahua Chemical Co., Ltd. with the model of EL-30; the sorbitol monopalmitate is purchased from Jiangsu Hai'an Petrochemical Plant with the model of S-40; the sodium dodecylbenzene sulfonate is purchased from Langfang Pengcai Fine Chemical Co., Ltd.; the thickener is polyvinyl alcohol; the antifreeze agent is glycerol; the organic solvent is 150 #solvent oil; and the water is deionized water.

[0065] The preparation method of the water emulsion is as follows:

[0066] (1) Dissolve the herbicidal composition in an organic solvent, add an emulsifier and stir evenly to obtain an oil phase;

[0067] (2) Mix a thickener and an antifreeze agent with water to obtain a water phase;

[0068] (3) Slowly add the oil phase into the water phase under the condition of high-speed shear, and continue to shear for 40 min to obtain the water emulsion.

Embodiment 3

[0069] Embodiment 3 provides a water emulsion of herbicial composition, which is prepared by the raw materials comprising the following components by weight percentage: herbicidal composition 12%, emulsifier 8%, thickener 5%, antifreeze agent 3%, organic solvent 24% and water (the residual percentage);

[0070] The herbicidal composition is a combination of benzylazole and nicosulfuron with a weight ratio of 1:50; the emulsifier is a combination of castor oil polyoxyethylene ether, sorbitol monopalmitate and sodium dodecylbenzene sulfonate with a weight ratio of 20:5:1; the castor oil polyoxyethylene ether is purchased from Jiahua Chemical Co., Ltd. with the model of EL-30; the sorbitol monopalmitate is purchased from Jiangsu Hai'an Petrochemical Plant with the model of S-40; the sodium dodecylbenzene sulfonate is purchased from Langfang Pengcai Fine Chemical Co., Ltd.; the thickener is polyvinyl alcohol; the antifreeze agent is glycerol; the organic solvent is 150 #solvent oil; and the water is deionized water.

[0071] The preparation method of the water emulsion is as follows:

[0072] (1) Dissolve the herbicidal composition in an organic solvent, add an emulsifier and stir evenly to obtain an oil phase;

[0073] (2) Mix a thickener and an antifreeze agent with water to obtain a water phase;

[0074] (3) Slowly add the oil phase into the water phase under the condition of high-speed shear, and continue to shear for 40 min to obtain the water emulsion.

Embodiment 4

[0075] The difference between embodiment 4 and embodiment 1 is that the emulsifier does not include castor oil polyoxyethylene ether.

Embodiment 5

[0076] The difference between embodiment 5 and embodiment 1 is that the castor oil polyoxyethylene ether is replaced with nonylphenol polyoxyethylene ether which is purchased from Nantong Runfeng Petrochemical Co., Ltd.

Embodiment 6

[0077] The difference between embodiment 6 and embodiment 1 is that the emulsifier does not include sorbitol monopalmitate.

Embodiment 7

[0078] The difference between embodiment 7 and embodiment 1 is that the emulsifier does not include sodium dodecylbenzene sulfonate,

Embodiment 8

[0079] The difference between embodiment 8 and embodiment 1 is that the thickner is xanthan gum.

Embodiment 9

[0080] The difference between embodiment 9 and embodiment 1 is that the solvent is dimethylformamide.

Embodiment 10

[0081] The difference between embodiment 10 and embodiment 1 is that the weight ratio of the solvent to emulsifier is 10:1.

Embodiment 11

[0082] The difference between embodiment 11 and embodiment 1 is that the herbicidal composition is the combination of benzylazole and acetochlor with a weight ratio of 1:30.

[0083] Performance Test

[0084] 1. Heat storage stability test: put the water emulsion in the same well-sealed scale test tubes respectively with a plug, and then store them in a 54±0.1° C. water bath for 14 days; the acceptance criteria are as follows: the system is homogeneous and the water precipitation rate is less than 10%.

[0085] 2. Cold store stability test: put the water emulsion in a scale test tube with a plug, then freeze it in the refrigerator at −18° C. for 24 h, then let it melt automatically under room temperature, and then put it in the refrigerator, and repeat this process for ten times; the acceptance criteria are as follows: no oil phase is separated out.

[0086] 3. Determination of emulsification stability: dilute the water emulsion 200 times with 342 ppm standard hard water, put it in a constant temperature water bath at 30° C. for 1 h, and take it out; observe the separation of emulsion; the acceptance criteria are as follows: no oil slick on the top and no sediment on the bottom.

[0087] See Table 1 for the performance test results of the embodiments.

TABLE-US-00001 TABLE 1 Performance test results of the embodiments Heat storage Cold Store Emulsification Embodiment stability stability stability Embodiment 1 Passed Passed Passed Embodiment 2 Passed Passed Passed Embodiment 3 Passed Passed Passed Embodiment 4 Failed Failed Failed Embodiment 5 Failed Failed Failed Embodiment 6 Failed Failed Failed Embodiment 7 Failed Failed Failed Embodiment 8 Failed Failed Failed Embodiment 9 Failed Failed Failed Embodiment 10 Failed Failed Failed Embodiment 11 Passed Passed Passed

[0088] 4. Control Effect Test:

[0089] Samples for test:

[0090] 95% benzylazole technical, 81.5% acetochlor EC

[0091] Crop:

[0092] Corn: conventional varieties planted in large areas in the market (Tiegan 505, Kejujia 23)

[0093] Weeds:

[0094] Annual weeds such as piemarker, goosefoots, Commelina communis, Amaranthus retroflexus, Solanum nigrum, wild watermelon seedlings, purslane, acalypha copperleaf, Xanthium sibiricum, Conyza canadensis, Eleusine indica, Eriochloa villosa, green bristlegrass, Echinochloa crusgalli, Alopecurus aequalis, Avena fatua, Poa annua, giant foxtail, etc.

[0095] Application method:

[0096] Mixed with 45 kg of water per mu, sprayed to soil (apply the pesticide 24 h after corns and weed seeds were sown together)

[0097] Statistical analysis method of test results:

[0098] Calculation of ED.sub.50/ED.sub.90 value of test agent

[0099] Calculated with DPS statistical analysis software

[0100] Calculation of Co-toxicity coefficient:

[00001]$\mathrm{Co}-\mathrm{toxicity}\mathrm{coefficient}=\frac{1/{\mathrm{ED}}_{50\left(90\right)}\mathrm{value}\mathrm{of}\mathrm{mixture}\mathrm{agent}}{P_A/{\mathrm{ED}}_{50\left(90\right)}\mathrm{value}\mathrm{of}\mathrm{agent}A+P_B/{\mathrm{ED}}_{50\left(90\right)}\mathrm{value}\mathrm{of}\mathrm{agent}B}*100$

[0101] Wherein: P.sub.A is the proportion of agent A in the effective components of the mixture, P.sub.B is the proportion of agent B in the effective components of the mixture, and if the co-toxicity coefficient is less than 80, it is an antagonistic effect; if the co-toxicity coefficient is greater than 120, it is a synergistic effect; and if the co-toxicity coefficient is between 80-120, it is an additive effect.

[0102] The results are shown in Table 2, in which A is 95% benzylazole technical and B is 81.5% acetochlor EC.

[0103] The results are as follows: the test agents in Table 2 (percentage conversion) refer to those calculated by being converted into 100% benzylazole and 100% acetochlor, for example, when the weight ratio of 95% benzylazole technical to 81.5% acetochlor EC is 1:90, the value obtained by percentage conversion is 1:77.

TABLE-US-00002 TABLE 2 Summary of efficacy results of test agents with different proportions Test agent ED.sub.50 (percentage value Co-toxicity Mixture conversion) (g a.i./hm.sup.2) A B A + B P.sub.A P.sub.B Coefficient Result A:B = 1:77 98.2 1 90 91 0.0110 0.9890 98 + A:B = 1:68 88.4 1 80 81 0.0123 0.9877 108 + A:B = 1:60 80.1 1 70 71 0.0141 0.9859 117 + A:B = 1:51 73.2 1 60 61 0.0164 0.9836 126 ++ A:B = 1:42 63.9 1 50 51 0.0196 0.9804 140 ++ A:B = 1:34 62.5 1 40 41 0.0244 0.9756 138 ++ A:B = 1:25 60.3 1 30 31 0.0323 0.9677 135 ++ A:B = 1:17 60 1 20 21 0.0476 0.9524 122 ++ A:B = 1:8 59 1 10 11 0.0909 0.9091 96 + A 10 B 106.7

[0104] Remarks: ED.sub.50 is the activity test result of Echinochloa crusgalli after 15 days of treatment with different agents

[0105] 5. Field Efficacy Test:

[0106] Test agent:

Embodiment 1 Water Emulsion of Herbicidal Composition

[0107] Control agent:

[0108] 10% benzylazole water emulsion (Nantong Jiangshan Pesticide Chemical Co., Ltd.), 81.5% acetochlor emulsion (Nantong Jiangshan Pesticide Chemical Co., Ltd.)

[0109] Crops for test:

[0110] Corn (Suyunuo No.11)

[0111] Controlled object:

[0112] Annual weeds (Echinochloa, Eleusine indica, purslane, Eclipta prostrata, Acalypha copperleaf, etc.)

[0113] Test method:

[0114] Cell division: the area of cells was 20 m.sup.2, and the cells were arranged randomly, and each cell was treated for 3 times.

[0115] Usage: mixed with 45 kg of water per mu and sprayed evenly on the ground surface before corn sowing.

[0116] Methods of Investigation, Recording and Measurement

[0117] Meteorological data: the weather on the test day was fine and breezy, and the temperature was normal and the efficacy was basically normal during the test.

[0118] Field management data: base fertilizer: 45%, compound fertilizer: 50 kg/mu. Other field management such as disease and insect prevention and topdressing were carried out according to normal management.

[0119] Weed investigation: the total weed control effect was visually investigated on the 7th, 10th, 15th, 30th and 45th days after application.

[0120] Investigation method: visual inspection.

[0121] Efficacy calculation method: the relative control effect percentage by visual inspection was recorded.

[0122] Crop investigation: visually observed the seedling emergence after corn sowing; the numbers of seedling emergence were investigated three times on the 4th, 7th and 12th days after sowing; and the growth of corn was observed on the 32nd and 47th days after sowing.

[0123] Investigation method: 20 seedlings for each treatment, and the safety degree of different doses on corn was observed.

[0124] The investigation results of the efficacy of the insecticide against weeds are as follows:

TABLE-US-00003 TABLE 3 Summary of effectiveness investigation of embodiment 1 on weeds Preparation consumption Effectiveness of annual weeds (%) Treatment agent (ml/mu) 7 days 10 days 15 days 30 days 45 days Embodiment 1 150 100 100 98 93 90 Water emulsion of herbicidal composition 10% 30 97 97 93 85 45 benzylazole water emulsion 81.5% 150 98 98 92 85 40 acetochlor EC Clear water for 0 15-20 35-40 350-550 550-850 850-1350 control seedlings/m.sup.2 seedlings/m.sup.2 seedlings/m.sup.2 seedlings/m.sup.2 seedlings/m.sup.2

[0125] The investigation results of the safety of the insecticide against crops are as follows:

TABLE-US-00004 TABLE 4 Summary of safety investigation of embodiment 1 on crops Number of emerging seedlings Corn growth (compared Preparation (%) (100 seeds) with the control group) Treatment consumption 4 d after 7 d after 12 d after 32 d after 47 d after agent (ml/mu) application application application application application Embodiment 150 95 94 94 The seedlings The seedlings 1 Water grow grow emulsion of normally normally herbicidal composition 10% 30 94 90 89 The seedlings The seedlings benzylazole grow grow water normally normally emulsion 81.5% 150 93 92 92 The seedlings The seedlings acetochlor grow grow EC normally normally Clear water 0 93 92 91 The seedlings The seedlings Control grow grow normally normally

[0126] The embodiments above are only illustrative and used to explain some features of the method described in the invention. The claims intend to claim the widest possible scope that can be envisaged, and the embodiments presented herein are only selected for illustration according to all possible combinations of embodiments. Therefore, it is the object of the applicant that the claims are not limited by the embodiments illustrating the features of the invention. Some numerical ranges used in the claims also include sub-ranges within them, and any changes in these ranges should also be covered by the claims where possible.