Weeding composition containing penoxsulam and oxadiazon and application thereof

Abstract

The invention belongs to the field of pesticides, and particularly relates to a weeding composition containing penoxsulam and oxadiazon and application thereof.The weeding composition is prepared from, by weight, 0.6%-1.2% of penoxsulam, 20%-24% of oxadiazon, 8%-16% of pesticide emulsifier 605, 1%-5% of Etherlan NS 500LQ, 0.5%-2% of SVA-116B, 0.15%-0.25% of ammonia water, 0.5%-2% of an antioxidant, 3%-7% of cyclohexanone, 4%-6% of ethylene glycol, 1%-2% of N, N-dimethyl formamide and the balance water. 30-40% of N, N-dimethylacetamide, and the balance of s-150. The missible oil preparation prepared by the invention has the advantages of high preparation stability, low raw medicine decomposition rate and excellent closed weeding effect.

Description

Technical Field

[0001] The present invention belongs to the field of pesticides, and particularly relates to a herbicidal composition containing penoxsulam and oxadiazon and its application. Background Art

[0002] Penoxsulam is a sulfonylurea herbicide, which is absorbed by the young buds, stems and leaves, and roots of weeds, and is conducted to the meristem through the xylem and phloem, inhibiting plant growth, yellowing until death. It can be used to control barnyard grass, annual sedges and some broad-leaved weeds in paddy fields.

[0003] Oxadiazon is a selective pre-emergence and post-emergence herbicide. It contacts, absorbs and accumulates in the vigorously growing parts through the young buds or seedlings of weeds, inhibits growth, and causes the weed tissues to rot and die. After application in paddy fields, the liquid medicine quickly spreads on the water surface and is rapidly adsorbed by the soil, forming a closed medicine film to prevent weed growth.

[0004] The patent application CN104186502A of Guangdong Zhongxun Agrochemical Co., Ltd. discloses a herbicidal composition containing oxadiazon and penoxsulam, which includes the active ingredients oxadiazon and penoxsulam, and the rest are pesticide adjuvants. The mass ratio of oxadiazon to penoxsulam is 1:1 to 140:1. Compared with the single agent used alone, it significantly improves the herbicidal effect, expands the weed control spectrum, is safe for crops, reduces the amount of pesticide used, reduces the environmental pollution of pesticides, and delays the emergence of weed resistance. And the disclosed dosage forms are one of suspension concentrates, oil suspension concentrates, water dispersible granules, wettable powders, effervescent tablets, and effervescent granules. The pesticide registration certificate PD20212842 of Anhui Kelihua Chemical Co., Ltd. discloses that 15% oxadiazon·penoxsulam suspension concentrate (1% penoxsulam, 14% oxadiazon) can be used for the control of annual weeds in transplanted paddy fields. There is no research and development on the emulsifiable concentrate preparation of penoxsulam and oxadiazon in the prior art.

[0005] Emulsifiable concentrate (EC) is an oily homogeneous liquid dosage form that can be dispersed into an emulsion after entering water. The processing equipment for emulsifiable concentrates is simple, and the formulation technology is easy to master, that is, the technical drug is dissolved in an organic solvent and then an emulsifier is added, and the three are mutually soluble. The emulsifiable concentrate has a high content of active ingredients, generally good stability, high drug efficacy, and convenient use. Through the research and screening of the emulsifiable concentrate formulation, the present invention has selected an emulsifiable concentrate with high formulation stability, low decomposition rate of the technical drug, and excellent closed herbicidal effect. Summary of the Invention

[0006] The present invention provides a herbicidal composition containing penoxsulam and oxadiazon and its application. The specific technical solutions are as follows:

[0007] A herbicidal composition containing penoxsulam and oxadiazon, characterized in that it contains the following components in weight percentages: penoxsulam 0.6 - 1.2%, oxadiazon 20 - 24%, agricultural emulsifier 605 8 - 16%, Ethylan NS 500LQ 1 - 5%, SVA - 116B 0.5 - 2%, ammonia water 0.15 - 0.25%, antioxidant 0.5 - 2%, cyclohexanone 3 - 7%, ethylene glycol 4 - 6%, N,N - dimethylacetamide 30 - 40%, s - 150 to make up 100.

[0008] The present invention provides a herbicidal composition containing penoxsulam and oxadiazon, which contains the following components in weight percentages: penoxsulam 0.6 - 1%, oxadiazon 21 - 23%, agricultural emulsifier 605 8 - 16%, Ethylan NS 500LQ 1 - 5%, SVA - 116B 0.5 - 2%, ammonia water 0.15 - 0.25%, antioxidant 0.5 - 2%, cyclohexanone 3 - 7%, ethylene glycol 4 - 6%, N,N - dimethylacetamide 30 - 40%, s - 150 to make up 100.

[0009] The present invention provides a herbicidal composition containing penoxsulam and oxadiazon, which contains the following components in weight percentages: penoxsulam 0.8%, oxadiazon 21.2%, agricultural emulsifier 605 12%, Ethylan NS 500LQ 3%, SVA - 116B 1%, ammonia water 0.2%, antioxidant 1%, cyclohexanone 5%, ethylene glycol 5%, N,N - dimethylacetamide 35%, s - 150 to make up 100.

[0010] The use of the herbicidal composition provided by the present invention for controlling crop weeds. The crop is rice, and the weeds are annual gramineous and broad - leaf weeds.

[0011] Compared with the prior art, the present invention has the following beneficial effects:

[0012] Ethylan NS 500LQ is emulsified with agricultural emulsifier 605 without precipitation, and the emulsion stability is qualified; when combined with various 5% alcohols, there is no floating oil with ethylene glycol; under normal circumstances, about 7% of penoxsulam decomposes after heat storage. Adding 1% antioxidant can control the decomposition rate at about 3%. Continuing to increase the antioxidant, the decomposition rate has no improvement. Adding 0.2% ammonia water to control the pH between 6.0 - 7.0, the decomposition rate of penoxsulam is below 1%.

[0013] Different from the traditional emulsifiable concentrate that disperses immediately when entering water, this product adds a thickener SVA - 116B, making the preparation viscous. After entering water, it will first sink to the bottom and then disperse, playing a role in closed weeding. Description of the Drawings

[0014] Figure 1: The sedimentation situation of the emulsion at 5 min of sedimentation;

[0015] Figure 2 : The sedimentation situation of the emulsion at 1 h of sedimentation;

[0016] Figure 3 : The sedimentation situation of the emulsion at 6 h of sedimentation;

[0017] Figure 4 : The sedimentation situation of the emulsion at 24 h of sedimentation. Specific implementation mode

[0018] According to the following embodiments, the present invention can be better understood. However, those skilled in the art can easily understand that the content described in the embodiments is only used to illustrate the present invention and should not and will not limit the present invention described in detail in the claims.

[0019] Example 1: Preparation of 22% penoxsulam and oxadiazon emulsifiable concentrate (EC) formulation

[0020] Main reagents: The reagents in the formulation table are all industrial products and are purchased from the market;

[0021] Main instruments: High performance liquid chromatograph (Agilent1100), shear emulsifying mixer, pH meter (Mettler), digital display constant temperature water bath, constant temperature forced air drying oven, electrothermal constant temperature incubator, freezer, electronic balance.

[0022] Preparation method: At room temperature, a certain amount of technical material is dissolved in an organic solvent, and the surfactant that has been ultrasonically fully mixed is added, and then stirred thoroughly for 300 min to mix evenly, and the emulsifiable concentrate can be obtained.

[0023] Detection method:

[0024] HPLC is used for the detection of the content of active ingredients;

[0025] The water content is determined by the Karl Fischer titration instrument determination method (GB / T1600 - 2001);

[0026] The calibration solution is prepared according to the instructions of the pH meter standard calibration reagent, and the pH meter is calibrated with reference to the method of GB / T1601 - 93.

[0027] The method for determining the emulsion stability is carried out according to the method of GB / T 1603-2001: Add 100 mL of standard hard water at 25-30 °C into a 250 mL beaker, suck 0.5 mL of the emulsifiable concentrate sample (diluted 20 times according to the national standard), and slowly add it to the hard water while stirring continuously. After adding the emulsifiable concentrate sample, continue to stir at a speed of 2-3 rps for 30 s. Immediately transfer the emulsion to a clean and dry 100 mL graduated cylinder, and place the graduated cylinder in a constant temperature water bath at (30±2) °C. Let it stand for 30 min and 1 h, and observe the separation of the emulsion. If there is no floating oil (paste), sediment oil or precipitation in the graduated cylinder, it is regarded as qualified for emulsion stability.

[0028] The evaluation method for the dispersibility and emulsification of the emulsifiable concentrate in water: Pour 99.5 mL of distilled water into a 100 mL graduated cylinder, and transfer 0.5 mL of the emulsifiable concentrate, and observe its dispersion state. After dropping the emulsifiable concentrate into the graduated cylinder, cover it with a stopper, turn the graduated cylinder 15 times, and observe the initial emulsion state.

[0029] The method for determining the low-temperature stability of the emulsifiable concentrate is carried out according to GB / T 19137-2003;

[0030] The method for determining the thermal storage stability of the emulsifiable concentrate is carried out according to GB / T 19136-2003;

[0031] The formulation of the emulsifiable concentrate preparation:

[0032] Table 1 Formulation table of 22% penoxsulam and oxadiazon emulsifiable concentrate EC

[0033]

[0034]

[0035] Table 2 Formulation table of 22% penoxsulam and oxadiazon emulsifiable concentrate EC (continued table)

[0036]

[0037] SVA-116B: Jiangsu Qingyu Chemical Technology Co., Ltd.; agricultural emulsion: Jiangsu Kaiyuan Technology Co., Ltd.

[0038] Test results and analysis:

[0039] As can be seen from Table 3, when Ethylan NS 500LQ is combined with agricultural emulsions 601, 602, 603, 604, and 605, the initial emulsification is all qualified. There is precipitation after half an hour when Ethylan NS 500LQ is combined with agricultural emulsions 601, 602, and 603, and there is precipitation after one hour when Ethylan NS 500LQ is combined with agricultural emulsion 604; there is no precipitation in the emulsification of Ethylan NS 500LQ combined with agricultural emulsion 605, and the emulsion stability is qualified.

[0040] One of the main purposes of emulsifiers is to improve the surface forces between the constituent phases in emulsifiable concentrates, enabling them to disperse evenly and stably in the system, that is, to reduce the interfacial tension. When emulsifier Ethylan NS 500LQ and emulsifier agricultural emulsion adjuvant 605 are used in combination and the dosage of emulsifier Ethylan NS 500LQ is greater than that of emulsifier agricultural emulsion adjuvant 605, a more superior synergistic effect is achieved, enabling better control of the hydrophilic-lipophilic balance value of the emulsifier.

[0041] Table 3 Evaluation of emulsion stability

[0042] Item Formulation 1 Formulation 2 Formulation 3 Formulation 4 Formulation 5 Formulation 6 Initial Qualified Qualified Qualified Qualified Qualified Qualified 30 min Qualified Qualified Precipitation Precipitation Precipitation Precipitation 1h Qualified Precipitation - - - -

[0043] As can be seen from Table 4, when the emulsifiable concentrate formulation is stored in a constant temperature oven at (54 ± 2) °C for 14 days, the decomposition rate of penoxsulam in Formulation 1 is 0.74%, and the decomposition rate of penoxsulam in Formulations 7 - 9 increases significantly.

[0044] Under normal circumstances, about 7% of penoxsulam decomposes after heat storage. Adding 1% antioxidant can control the decomposition rate at about 3.5%. In actual production, continuing to increase the antioxidant does not improve the decomposition rate. However, adding 0.2% ammonia water and controlling the pH value between 6.0 and 7.0 can keep the decomposition rate of penoxsulam below 1%, significantly improving the thermal stability of penoxsulam.

[0045] Table 4 Evaluation of the thermal stability of penoxsulam

[0046]

[0047] As can be seen from Table 5, when combined with 5% alcohols (ethylene glycol, glycerol, propylene glycol), there is no floating oil with ethylene glycol, while floating oil problems of varying degrees occur with glycerol and propylene glycol.

[0048] Table 5 Evaluation of emulsion stability

[0049]

[0050] As can be seen from Table 6, all quality indicators of 22% penoxsulam and oxadiazon emulsifiable concentrate meet the emulsifiable concentrate product standard.

[0051] Table 6 Performance indicators of 22% penoxsulam and oxadiazon emulsifiable concentrate

[0052]

[0053]

[0054] Example 2: Closed weeding effect of 22% penoxsulam and oxadiazon emulsifiable concentrate on weeds in transplanted rice fields

[0055] Experimental site: The experimental field is paddy soil with medium fertility, where rice is grown all year round;

[0056] Test agents: Formulation 1 and Formulation 12 in Implementation 1;

[0057] Test method: The test set up a treatment group and a control group, each treatment was repeated 4 times, the plot area was 25m2, and the plot was arranged randomly. After the experimental field was plowed, the ridges were made according to the set plot area. The ridge height was 15-20cm and the ridge width was about 15cm to ensure that there was no mutual leakage between the plots. A drainage ditch 50cm wide was left between the plots, and the irrigation and drainage were independent without cross-drainage. After the plot was irrigated, a 3cm shallow water layer was irrigated, and the agent was mixed with fine sand and soil at 20kg / mu and evenly applied; water was retained for 2-4 days after the drug was applied until the plot dried naturally and then transplanted.

[0058] Survey method: 4 points were randomly surveyed in each plot 30 days after spraying, and 0.25m2 sample plot was taken at each point. The fresh weight of weeds was investigated 30 days after spraying.

[0059] Control effect (%) = (CK-PT) / CK×100

[0060] Where: PT is the fresh weight of residual weeds in the treatment area, and CK is the fresh weight of live weeds in the blank control area.

[0061] Test results and analysis:

[0062] As shown in Table 7, unlike traditional emulsifiable concentrates that disperse immediately after entering water, this product adds SVA-116B to make the preparation sticky. After entering water, it will first sink to the bottom and then disperse, which significantly improves the closed weed control effect.

[0063] Table 7 The closed weeding effect of 22% penoxsulam and oxadiazon EC on weeds in rice transplant fields

[0064] Treatment Dosage of preparation (ml / mu) Field control effect Formulation 1 100 95.0 Formulation 12 100 89.8

[0065] Example 3: EC sedimentation test

[0066] Two 500ml beakers were prepared, each filled with 80ml soil and 400ml water, one of which was stirred (for simulating muddy water application), and the other was not stirred (for simulating clear water application); then 2ml of formula 1 emulsifiable concentrate was added to each beaker. It can be clearly observed that the emulsion quickly sank to the soil in the simulated clear water application, and the emulsion also sank quickly in the simulated muddy water application.

[0067] Then, the active ingredient content between 200 mL and 300 mL of the beaker was tested at 5 min, 1 h, 6 h and 24 h, as shown in Table 8 and the accompanying drawings.

[0068] Table 8: EC sedimentation test

[0069]

[0070] The above are only the preferred embodiments of the present invention. For those skilled in the art, without departing from the raw materials of the present invention, appropriate improvements can be made, and these improvements are also within the protection scope of the present invention.

Claims

1. A herbicidal composition comprising penoxsulam and oxadiazon, characterized in that: The invention comprises the following ingredients in percentage by weight: penoxsulam 0.6-1.2%, oxadiazon 20-24%, Nongru 6058-16%, Ethylan NS 500LQ1-5%, SVA-116B0.5-2%, ammonia water 0.15-0.25%, antioxidant 0.5-2%, cyclohexanone 3-7%, ethylene glycol 4-6%, N,N-dimethylacetamide 30-40%, and s-150 supplemented to 100.

2. The herbicidal composition according to claim 1, characterized in that The invention comprises the following ingredients in percentage by weight: penoxsulam 0.6-1%, oxadiazon 21-23%, agricultural milk 6058-16%, Ethylan NS 500LQ 1-5%, SVA-116B 0.5-2%, ammonia water 0.15-0.25%, antioxidant 0.5-2%, cyclohexanone 3-7%, ethylene glycol 4-6%, N,N-dimethylacetamide 30-40%, and s-150 supplemented to 100.

3. The herbicidal composition according to claim 1, characterized in that The invention comprises the following ingredients in percentage by weight: 0.8% of penoxsulam, 21.2% of oxadiazon, 12% of agricultural milk adjuvant 605, 3% of Ethylan NS 500LQ, 1% of SVA-116B, 0.2% of ammonia water, 1% of antioxidant, 5% of cyclohexanone, 5% of ethylene glycol, 35% of N,N-dimethylacetamide, and 100% of s-150.

4. Use of the herbicidal composition according to any one of claims 1 to 3 for controlling crop weeds.

5. The use according to claim 4, characterized in that The crop is rice, and the weeds are annual grasses and broad-leaved weeds.

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