阅读说明：本技术 一种含砜吡草唑与氯酯磺草胺的组合物及其应用 (Composition containing pyraflufen-ethyl and cloransulam-methyl and application thereof ) 是由 李志清 王建伟 雷艳林 孙鹏 于 2021-09-23 设计创作，主要内容包括：本发明公开了一种含砜吡草唑与氯酯磺草胺的组合物及其应用,砜吡草唑与氯酯磺草胺的质量比为1-10：1。本发明将药物活性成分砜吡草唑与氯酯磺草胺进行复配,本发明本发明该制剂扩大了除草谱,提高了药物持效期,延缓了抗药性产生,在防治大豆田一年及多年生杂草有很好的效果。本发明还提供了砜吡草唑与氯酯磺草胺的可湿性粉剂,该制剂制备过程简单,便于储存和运输,通过对助剂的优选,所得可湿性粉剂具有悬浮率高、热稳定性好、润湿时间短、起泡性低等优势,在不同的水质条件下均具有较好的悬浮率。(The invention discloses a composition containing pyraflufen-ethyl and cloransulam-methyl and application thereof, wherein the mass ratio of the pyraflufen-ethyl to the cloransulam-methyl is 1-10: 1. according to the invention, the active ingredients of the herbicide, namely the topramezone and the cloransulam-methyl, are compounded, so that the herbicide expands the weeding spectrum, improves the drug effect duration, delays the generation of drug resistance, and has a good effect of preventing and treating annual and perennial weeds in soybean fields. The invention also provides wettable powder of the topramezone and the cloransulam, the preparation process is simple, the storage and the transportation are convenient, and the obtained wettable powder has the advantages of high suspension rate, good thermal stability, short wetting time, low foamability and the like by optimizing the auxiliary agent, and has better suspension rate under different water quality conditions.)

1. The composition containing the topramezone and the cloransulam-methyl is characterized in that: the active ingredients of the medicine comprise the topramezone and the cloransulam-methyl, and the mass ratio of the topramezone to the cloransulam-methyl is 1-10: 1.

2. the composition as set forth in claim 1, characterized in that: the mass ratio of the xaflufen to the cloransulam-methyl is 3-7:1, preferably 5:1.

3. the composition according to claim 1 or 2, characterized in that: the content of the pharmaceutically active ingredient is 1 to 85wt%, preferably 20 to 85wt%, more preferably 50 to 80 wt%.

4. The composition according to any one of claims 1 to 3, characterized in that: the dosage form of the composition is wettable powder.

5. The composition as set forth in claim 4, wherein: the wettable powder consists of the following components in percentage by weight: 1-85% of active ingredients of the medicine, 6.0-10.0% of dispersing agent, 2.0-6.0% of wetting agent, 2.0-5.0% of stabilizing agent, 0.2-0.5% of pH regulator and the balance of filler.

6. The composition as set forth in claim 5, characterized in that: the dispersing agent is one or more of lignosulfonate, methyl naphthalene sulfonic acid formaldehyde condensate sulfate, naphthalene sulfonic acid formaldehyde condensate sodium salt, methylene sodium naphthalene sulfonate dibutyl naphthalene sulfonic acid formaldehyde condensate, N-methyl fatty acyl sodium taurate, alkyl naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate and sodium polycarboxylate; the wetting agent is one or more of sodium dodecyl sulfate, a-sulfo fatty acid methyl ester, sodium tetradecyl sulfate, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate, a-olefin sodium sulfonate, sodium alkylphenol polyoxyethylene ether sulfate, sodium diisobutyl naphthalene sulfonate, fatty acid sulfate and fatty acid ester sulfate; the stabilizer is one or more of microcrystalline cellulose, tricalcium phosphate, sodium aluminosilicate and white carbon black; the pH regulator is one or more of citric acid, sodium benzoate, sodium acetate and sodium hexametaphosphate; the filler is one or more of potassium sulfate, potassium chloride, diammonium hydrogen phosphate, anhydrous sodium sulfate, ammonium sulfate, kaolin, bentonite, talcum powder, attapulgite, diatomite, starch and light calcium carbonate.

7. The composition according to claim 5 or 6, characterized in that: the dispersing agent is formed by mixing sodium naphthalene sulfonate formaldehyde condensate and alkyl naphthalene sulfonate formaldehyde condensate according to the mass ratio of 2.0-3.0: 1.0; the wetting agent is formed by mixing sodium dodecyl sulfate and sodium alkyl naphthalene sulfonate according to the mass ratio of 1.0-1.5: 1.0; the stabilizer is white carbon black.

8. The composition according to claim 5 or 6, characterized in that: the pH regulator is citric acid; the filler is kaolin or a mixture of talcum powder and kaolin.

9. Use of a composition containing pyraflufen-ethyl and cloransulam as claimed in any one of claims 1 to 8 for controlling annual and perennial weeds in crops.

10. Use according to claim 9, characterized in that: the crops are soybeans and peanuts, the weeds are annual and perennial grassy weeds and annual and perennial broadleaf weeds, and the weeds are preferably hard ryegrass which has drug resistance due to continuous use of the pyraflufen-ethyl.

Technical Field

The invention relates to a composition containing pyraflufen-ethyl and cloransulam, and also relates to a formulation, a preparation method and application thereof in weeding, belonging to the technical field of pesticides.

Background

Pyraflufen-ethyl (Pyroxasulfone), chemical name: the 3- [5- (difluoromethoxy) -1-methyl-3- (trifluoromethyl) pyrazol-4-yl methylsulfonyl ] -4, 5-dihydro-5, 5-dimethyl-1, 2-isoxazole belongs to a novel isoxazole herbicide, is widely applied to crops, is mainly used for crops such as corn, cotton, peanut, wheat and sunflower, and can effectively prevent and kill gramineous weeds such as setaria, crabgrass and cockspur grass and broadleaf weeds such as amaranthus, stramonium, solanum and abutilon.

Cloransulam-methyl, chemical name: methyl 3-chloro-2- (5-ethoxy-7-fluoro [1,2,4] triazolo [1,5-c ] pyrimidine-2-yl sulfonyl) aminobenzoate belongs to sulfonamide herbicides and is mainly used for controlling broadleaf weeds by spraying stem leaves of soybean fields.

Herbicide varieties containing a single active component often have different degrees of defects in agricultural pest control, such as: the weeding spectrum is narrow, the weeds are easy to generate drug resistance after continuous use, the environmental pollution is aggravated after the weeds are used for many times, and researches show that the fenpyrazazole can be continuously and singly applied for three years, the hard ryegrass can generate resistance to the fenpyrazazole and even generate interactive resistance to other agents, and after the cloransulam-methyl is applied, the soybean leaves are easy to generate the symptom of chlorotic phytotoxicity and are easy to generate phytotoxicity to succeeding crops. Therefore, the method has important research significance on how to enable the topramezone and the cloransulam-methyl to have a better weeding effect and overcome the weed resistance and the damage to crops in the using process.

Disclosure of Invention

Aiming at the problems of drug resistance, phytotoxicity and the like of the existing single agents of the pyraflufen-ethyl and the cloransulam in the using process, the invention provides the composition containing the pyraflufen-ethyl and the cloransulam, the composition is prepared by compounding the pyraflufen-ethyl and the cloransulam, the two agents show obvious synergistic action, the weeding effect is improved, the drug use amount and the use times are reduced, the environmental pollution is reduced, the safety of the compounded composition on crops is improved, the residual phytotoxicity of the succeeding crops is reduced, and the drug resistance of weeds is delayed.

The specific technical scheme of the invention is as follows:

a composition containing pyroxsulam sulfone and cloransulam-methyl, wherein the active pharmaceutical ingredients in the composition comprise pyroxsulam sulfone and cloransulam-methyl, the mass ratio of the pyroxsulam sulfone to the cloransulam-methyl is 1-10: 1.

furthermore, the active pharmaceutical ingredients in the composition can be only two of the sulfuryl pyraoxystrobin and the cloransulam-methyl, or can be active pharmaceutical ingredients containing the two. When the ratio of the topramezone to the cloransulam-methyl is 1-10: 1, the composition can play a good role in drug synergism, reduce the usage amount of the drug and improve the drug effect.

Preferably, the mass ratio of the xaflufen to the cloransulam is 3-7:1, more preferably 5:1. within the range, the compound of the pyraflufen-ethyl and the cloransulam can play a better role.

Further, the content of the pharmaceutically active ingredient in the above composition is 1 to 85wt%, preferably 20 to 85wt%, more preferably 50 to 80 wt%.

Furthermore, the composition can be prepared into various appropriate dosage forms according to the guidance of the prior art, such as wettable powder, water dispersible granules, suspending agents and the like. The formulation and preparation of each formulation can be found in the prior art.

Further, the bulk drug of the sulfuryl pyraoxystrobin is white solid, and the water distribution coefficient of n-octanol/water is as follows: logP 2.39 (pH: 8.7, 25 ℃), cloransulam technical as a white solid, coefficient of n-octanol/water partition: logP ═ 1.12(25 ℃), both active ingredients being relatively hydrophilic technical materials. When the topramezone and the cloransulam-methyl are used as the active pharmaceutical ingredients, the problems of agglomeration due to pressurization and heat storage, low suspension rate, slow wetting time, high foamability and the like exist when the topramezone and the cloransulam-methyl are prepared into wettable powder. The invention aims at the problems, researches and screens the auxiliary agent of the wettable powder, solves the problems by selecting and matching the dispersing agent, the wetting agent and the stabilizing agent, obtains the wettable powder with excellent performance and better pharmacodynamic performance, can better exert the pharmacodynamic action of the active ingredients of the medicament, has good weed control effect, can expand the weeding spectrum, improves the safety of crops and reduces the residual phytotoxicity of afterreap, and has simple manufacturing process and convenient storage and transportation.

Further, the preferable wettable powder formulation of the invention is (weight percentage): 1-85% of active ingredients of the medicine, 6.0-10.0% of dispersing agent, 2.0-6.0% of wetting agent, 2.0-5.0% of stabilizing agent, 0.2-0.5% of pH regulator and the balance of filler. The active ingredients of the medicine are the above-mentioned sulfurazol and cloransulam, and the mass ratio of the sulfurazol to the cloransulam is 1-10: 1, preferably 3-7:1, more preferably 5:1.

Furthermore, the components of the wettable powder preferably adopt the following weight percentage: 20-85% of active ingredients of the medicine, 6.0-10.0% of dispersing agent, 2.0-6.0% of wetting agent, 2.0-5.0% of stabilizing agent, 0.2-0.5% of pH regulator and the balance of filler.

Furthermore, the components of the wettable powder preferably adopt the following weight percentage: 50-80% of active ingredients of the medicine, 6.0-10.0% of dispersing agent, 2.0-6.0% of wetting agent, 2.0-5.0% of stabilizing agent, 0.2-0.5% of pH regulator and the balance of filler.

Furthermore, in the above wettable powder, a dispersant, a wetting agent, a stabilizer, a pH adjuster, and a filler are collectively referred to as an aid, and the dispersant functions to prevent fine particles of the pharmaceutically active ingredient from aggregating with each other and keep them uniformly dispersed for a long time in a liquid-solid dispersion system formed with water. The wetting agent functions to reduce the liquid-solid surface tension of the fine particles in water, increasing the ability to be wetted by water. The stabilizer and the pH regulator function to prevent agglomeration of the powder and decomposition of the pharmaceutically active ingredient during long-term storage. The filler is used for loading or diluting the active ingredients of the medicine and adjusting the content of the product to reach the standard.

Further, the dispersant is one or a mixture of lignosulfonate, methyl naphthalene sulfonic acid formaldehyde condensate sulfate, naphthalene sulfonic acid formaldehyde condensate sodium salt, methylene naphthalene sulfonic acid sodium dibutyl naphthalene sulfonic acid formaldehyde condensate, N-methyl fatty acyl sodium taurate, alkyl naphthalene sulfonic acid formaldehyde condensate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate and polycarboxylic acid sodium.

Further, the wetting agent is one or more of sodium dodecyl sulfate, a-sulfo fatty acid methyl ester, tetradecyl sodium sulfate, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate, sodium a-olefin sulfonate, sodium alkylphenol polyoxyethylene ether sulfate, sodium diisobutyl naphthalene sulfonate, fatty acid sulfate and fatty acid ester sulfate.

Further, the stabilizer is one or more of microcrystalline cellulose, tricalcium phosphate, sodium aluminosilicate and white carbon black.

Further, the pH regulator is one or more of citric acid, sodium benzoate, sodium acetate, sodium hexametaphosphate and the like.

Further, the filler is one or more of potassium sulfate, potassium chloride, diammonium hydrogen phosphate, anhydrous sodium sulfate, ammonium sulfate, kaolin, bentonite, talcum powder, attapulgite, diatomite, starch and light calcium carbonate.

Furthermore, tests show that when the following preferable additives are selected as the additives, the suspension rate, the wetting time, the lasting foamability and the heat storage stability of the wettable powder are greatly improved, and the pesticide effect is also improved to a certain extent. Preferably, the dispersing agent is formed by mixing sodium salt of naphthalene sulfonic acid formaldehyde condensate and alkyl naphthalene sulfonate formaldehyde condensate according to the mass ratio of 2.0-3.0: 1.0; the wetting agent is formed by mixing sodium dodecyl sulfate and sodium alkyl naphthalene sulfonate according to the mass ratio of 1.0-1.5: 1.0; the stabilizer is white carbon black; the pH regulator is citric acid; the filler is kaolin, or a mixture of talc and kaolin.

Furthermore, when talcum powder and kaolin are selected as fillers, the content of the talcum powder is 5-10% of the wettable powder, and the kaolin is complemented to 100%.

The preparation method of the wettable powder is simple, and the finished product of the wettable powder can be obtained by uniformly mixing the pyraflufen-ethyl, the cloransulam, the dispersing agent, the wetting agent, the stabilizing agent, the pH regulator and the filler in a mixer, crushing the mixture to the particle size of 15-20 mu m by an airflow crusher and then uniformly mixing the mixture.

The composition containing the topramezone and the cloransulam-methyl and the preparation thereof expand the weeding spectrum, improve the control effect of the medicament, improve the lasting period of the medicament, reduce the dosage, delay the generation of medicament resistance, have higher control effect than a single dose, are safer to crops and are more beneficial to practical application. The composition and the preparation have good application prospect in preventing and controlling annual and perennial weeds of crops, wherein the crops can be soybeans, peanuts and the like, and the weeds can be annual and perennial gramineous weeds, annual and perennial broadleaf weeds, such as crabgrass, cockspur grass, dayflower, piemarker, glehnia littoralis, endive, lolium durum and the like. In particular, the herbicide composition has good control effect on annual and perennial weeds in soybean fields, and hard ryegrass which generates drug resistance when the pyraflufen-ethyl is continuously used.

The invention has the following beneficial effects:

1. the composition expands the weeding spectrum, improves the control effect of the medicament, improves the duration of the medicament, reduces the dosage, is more beneficial to practical application, and is particularly suitable for controlling annual and perennial weeds of soybeans.

2. According to the invention, the active ingredients of the herbicide comprising the topramezone and the cloransulam-methyl are compounded, so that the problem of the drug resistance of the hard ryegrass caused by the continuous use of the single topramezone is solved, the phytotoxicity of the application of the topramezone to the soybeans is also solved, the safety of the herbicide is improved, the residual phytotoxicity of the succeeding crops is reduced, the generation of the drug resistance is delayed, and the sustainable development of the environment is facilitated.

3. The invention prepares the sulfuryl pyraflufen and the cloransulam to wettable powder, has simple preparation process and is convenient for storage and transportation. By optimizing the auxiliary agent, the obtained wettable powder has the advantages of high suspension rate, good thermal stability, short wetting time, low foamability and the like, and has better suspension rate under different water quality conditions.

Detailed Description

The present invention is further illustrated by the following specific examples, which are merely illustrative of the present invention so as to enable those skilled in the art to better understand the present invention, but the essence of the present invention is not limited to the following examples.

The embodiment of the invention adopts a method combining indoor toxicity measurement and field test. Firstly, evaluating the joint action mode of the binary herbicides according to a Sun Yunpei co-toxicity coefficient method, defining the co-toxicity coefficient (CTC) of the two medicaments compounded according to a certain proportion, wherein the CTC is less than 80 and is antagonistic, the CTC is more than or equal to 80 and is less than or equal to 120 and is additive, and the CTC is more than 120 and is synergistic, and then carrying out field tests on the basis.

Indoor toxicity determination of toprament by compounding pyraflufen-ethyl and cloransulam

The indoor toxicity assay was as follows:

the test agents were provided by Shandong Weifang Runfeng Feng chemical company Limited.

And (3) experimental design: after the effective inhibition concentration range of each medicament is determined through pre-test, each medicament is respectively treated with a series of concentrations according to the content of effective components, and clear water is used for comparison. The test material is cultured in a climatic chamber at a temperature of 25-35 ℃. Sowing a certain amount of piemarker seeds into a plastic basin with the diameter of 9cm, covering soil for 1-2 mm, putting the piemarker seeds into an enamel tray filled with water, allowing the water to gradually permeate, spraying the liquid medicine when the piemarker grows to 2-4 leaves, and transferring the liquid medicine into a phytotron for later use after treatment. Weighing the fresh weight of the overground part of each treated weed 30 days after the application of the herbicide, and calculating the fresh weight control effect and ED₅₀The co-toxicity coefficient was calculated by the method proposed by Sun Yunpei et al (1960).

The calculation formula is as follows (taking cloransulam-methyl as a standard medicament and the virulence index thereof is 100)

Theoretical virulence index (TTI) of M-cloransulam-methyl TI XP_{Cloransulam-methyl}+ Sulfuron pyrazoxazole TI XP_Sulfoxaden

In the formula: m is a mixture of cloransulam-methyl and pyraflufen-ethyl in different proportions;

P_{cloransulam-methyl}Is the proportion of cloransulam-methyl in the mixture;

P_sulfoxadenIs the proportion of the sultopyrazole in the mixture.

The test results are shown in table 1:

TABLE 1 measurement of the Activity of Sulfoxaden and cloransulam under different formulation ratios to Abutilon

As can be seen from the above table, ED of cloransulam-methyl, pyriftalid against abutilon₅₀Are respectively 10.25g a.i/hm²And 22.52g a.i/hm². The mixture ratio of cloransulam-methyl to the xaflufen-ethyl is 1:15, the cotoxicity coefficient is 92.09, is more than 80 but less than 120, and the cloransulam-methyl and the xaflufen-ethyl are shown to be additive; the co-toxicity coefficients of the mixture ratio of 1:1, 1:3, 1:5, 1:7 and 1:10 are respectively 122.93, 133.25, 141.15, 134.75 and 121.21 which are all larger than 120, and the synergistic effect is shown, wherein the mixture ratio of cloransulam to xaflufen is 1: the synergistic effect is better when the ratio is 3-7, and the synergistic effect is best when the ratio is 1: 5.

Several examples of wettable powders of the invention are specifically set forth below to further demonstrate the advantages of the invention, but the invention is not limited thereto. Unless otherwise specified, the percentages in the following examples are by weight.

Example 121% wettable powder of Sulfoxaden-cloransulam

The formula is as follows: 17% of sulfonylpyraflufen, 4% of cloransulam, 2.0% of dispersant methyl naphthalene sulfonic acid formaldehyde condensate sulfate, 4.0% of methylene sodium naphthalene sulfonate dibutyl naphthalene sulfonic acid formaldehyde condensate, 1.0% of wetting agent a-sulfo fatty acid methyl ester, 1.5% of sodium dodecyl sulfate, 2.5% of stabilizing agent tricalcium phosphate, 0.2% of pH regulator citric acid, 25% of filler bentonite and 100% of potassium chloride.

The preparation method comprises the following steps: uniformly mixing the sulfurpyraflufen, the cloransulam, the dispersing agent, the wetting agent, the stabilizing agent and the filler in a mixer, crushing the mixture to be 15-20 mu m in particle size by an airflow crusher, mixing the mixture for the second time, and uniformly mixing the mixture to obtain the sulfurpyraflufen-cloransulam wettable powder.

Example 231% wettable powder of sulfonylpyraflufen

The formula is as follows: 20% of pyraflufen-ethyl, 11% of cloransulam, 6.0% of sodium polycarboxylate serving as a dispersant, 4.0% of sodium salt of a naphthalene sulfonic acid formaldehyde condensate, 1.5% of sodium alkylphenol polyoxyethylene ether sulfate serving as a wetting agent, 1.0% of sodium dodecyl benzene sulfonate, 2.5% of sodium aluminosilicate serving as a stabilizer, 0.4% of sodium benzoate serving as a pH regulator, 25% of talcum powder serving as a filler and light calcium carbonate which are added to 100%. The preparation method is the same as example 1.

Example 380% wettable powder of Sulfoxaden-cloransulam

The formula is as follows: 70% of sulfonylpyraflufen, 10% of cloransulam, 4.0% of sodium polycarboxylate serving as a dispersant, 4.0% of sodium salt of a naphthalene sulfonic acid formaldehyde condensate, 2.0% of sodium alkylphenol polyoxyethylene ether sulfate serving as a wetting agent, 1.0% of sodium alpha-olefin sulfonate, 3.0% of white carbon black serving as a stabilizer, 0.5% of sodium acetate serving as a pH regulator and 100% of kaolin serving as a filler.

The preparation method is the same as example 1.

Example 480% wettable powder of Sulfoxaden-cloransulam

The formula is as follows: 60% of pyraflufen-ethyl, 20% of cloransulam, 8% of dispersant sodium lignosulfonate, 2.0% of N-methyl fatty acyl sodium taurate, 3.5% of wetting agent sodium dodecyl benzene sulfonate, 2.0% of diisobutyl naphthalene sulfonate, 3% of stabilizer microcrystalline cellulose, 0.5% of pH regulator sodium benzoate and 100% of filler attapulgite.

The preparation method is the same as example 1.

Example 580% wettable powder of sulfonylpyraflufen-cloransulam

The formula is as follows: 67% of sulfonylpyraflufen, 13% of cloransulam, 5.0% of dispersant sodium lignosulfonate, 2.0% of alkyl naphthalene sulfonate formaldehyde condensate, 1.5% of wetting agent sodium alkyl naphthalene sulfonate, 1.0% of sodium dodecyl sulfate, 3% of stabilizer tricalcium phosphate, 0.5% of pH regulator citric acid and 100% of filler kaolin.

The preparation method is the same as example 1.

Example 680% wettable powder of sulfonylpyraflufen-cloransulam

The formula is as follows: 67% of sulfonylpyraflufen, 13% of cloransulam, 4.5% of a dispersant naphthalene sulfonic acid formaldehyde condensate sodium salt, 2.0% of an alkyl naphthalene sulfonate formaldehyde condensate, 1.0% of a wetting agent alkyl naphthalene sulfonic acid sodium salt, 1.0% of sodium dodecyl sulfate, 3.5% of a stabilizer common white carbon black, 0.5% of a pH regulator citric acid and kaolin added to 100% as a filler.

The preparation method is the same as example 1.

Example 755% Sulfoxaden cloransulam wettable powder

The formula is as follows: 48 percent of sulfonylpyraflufen, 7 percent of cloransulam, 5.0 percent of dispersant naphthalene sulfonic acid formaldehyde condensate sodium salt, 5.0 percent of alkyl naphthalene sulfonate formaldehyde condensate, 3.0 percent of wetting agent alkyl naphthalene sulfonic acid sodium salt, 3.0 percent of sodium dodecyl sulfate, 4.0 percent of stabilizer common white carbon black, 0.5 percent of pH regulator citric acid, 10 percent of filler talcum powder and 100 percent of kaolin.

The preparation method is the same as example 1.

Example 863% wettable powder of sulfonylpyraflufen-cloransulam

The formula is as follows: 52.5 percent of sulfonylpyraflufen, 10.5 percent of cloransulam, 3.0 percent of sodium salt of a naphthalene sulfonic acid formaldehyde condensate serving as a dispersant, 3.0 percent of an alkyl naphthalene sulfonate formaldehyde condensate, 1.0 percent of sodium alkyl naphthalene sulfonate serving as a wetting agent, 1.5 percent of sodium dodecyl sulfate, 5.0 percent of white carbon black serving as a stabilizer, 0.5 percent of citric acid serving as a pH regulator, 10 percent of filler talcum powder and 100 percent of kaolin.

The preparation method is the same as example 1.

Example 977% wettable powder of sulfonylpyraflufen-cloransulam

The formula is as follows: 64 percent of sulfonylpyraflufen, 13 percent of cloransulam, 3.0 percent of dispersant naphthalene sulfonic acid formaldehyde condensate sodium salt, 3.0 percent of alkyl naphthalene sulfonate formaldehyde condensate, 1.0 percent of wetting agent alkyl naphthalene sulfonic acid sodium salt, 1.5 percent of sodium dodecyl sulfate, 4.0 percent of stabilizer common white carbon black, 0.5 percent of pH regulator citric acid and 100 percent of filler kaolin.

The preparation method is the same as example 1.

Example 1080% wettable powder of Sulfoxaden-cloransulam

The formula is as follows: 67% of sulfonylpyraflufen, 13% of cloransulam, 5.0% of a dispersant naphthalene sulfonic acid formaldehyde condensate sodium salt, 2.5% of an alkyl naphthalene sulfonate formaldehyde condensate, 1.0% of a wetting agent alkyl naphthalene sulfonic acid sodium salt, 1.5% of sodium dodecyl sulfate, 3.5% of a stabilizer common white carbon black, 0.5% of a pH regulator sodium hexametaphosphate and 100% of filler anhydrous sodium sulfate.

The preparation method is the same as example 1.

Example 1130% wettable powder of Sulfoxaden-cloransulam

The formula is as follows: 25% of sulfonylpyraflufen, 5% of cloransulam, 4.0% of a dispersant naphthalene sulfonic acid formaldehyde condensate sodium salt, 2.0% of an alkyl naphthalene sulfonate formaldehyde condensate, 1.0% of a wetting agent alkyl naphthalene sulfonic acid sodium salt, 1.0% of sodium dodecyl sulfate, 3.0% of a stabilizer common white carbon black, 0.3% of a pH regulator citric acid and 100% of a filler added with kaolin.

The preparation method is the same as example 1.

Example 1280% wettable powder of Sulfenpyrad cloransulam

The formula is as follows: 70% of sulfonylpyraflufen, 10% of cloransulam, 4.5% of a dispersant naphthalene sulfonic acid formaldehyde condensate sodium salt, 2.0% of an alkyl naphthalene sulfonate formaldehyde condensate, 1.0% of a wetting agent alkyl naphthalene sulfonic acid sodium salt, 1.0% of sodium dodecyl sulfate, 3.5% of a stabilizer common white carbon black, 0.5% of a pH regulator citric acid and 100% of a filler added with kaolin.

The preparation method is the same as example 1.

Example 1380% wettable powder of sulfonylpyraflufen

The formula is as follows: 72 percent of sulfonylpyraflufen, 8 percent of cloransulam, 4.5 percent of dispersant naphthalene sulfonic acid formaldehyde condensate sodium salt, 2.0 percent of alkyl naphthalene sulfonate formaldehyde condensate, 1.0 percent of wetting agent alkyl naphthalene sulfonic acid sodium salt, 1.0 percent of sodium dodecyl sulfate, 3.5 percent of stabilizer common white carbon black, 0.5 percent of pH regulator citric acid and kaolin added to 100 percent of filler.

The preparation method is the same as example 1.

Comparative example 180% wettable powder of sulfonylpyraflufen-cloransulam

The formula is as follows: 67% of sulfonylpyraflufen, 13% of cloransulam, 4% of dispersant modified lignin, 3.5% of polyoxyethylene ether formaldehyde condensate, 1.5% of wetting agent nekal, 1.5% of sodium petroleum sulfonate, 3.0% of stabilizer common white carbon black, 0.5% of pH regulator citric acid and 100% of filler kaolin.

The preparation method is the same as example 1.

Quality result detection is carried out on the product quality indexes of the wettable powder preparation of the sulfuryl pyraoxystrobin and the cloransulam-methyl prepared in the above examples and comparative examples.

Wherein, the method for detecting the fineness of the wettable powder is CIPAC MT185, the method for detecting the suspension percentage is CIPAC MT15.1, the method for detecting the wetting time is CIPAC MT 53.3, and the method for detecting the heat storage stability is CIPAC MT 46.3. The results are shown in Table 2.

TABLE 2 wettable powder product quality index prepared by compounding pyraflufen-ethyl and cloransulam-methyl

As can be seen from the data in table 2, the suspension rate of the wettable powder prepared in examples 1 to 5 before heat storage reaches more than 85%, no fine powder exists after screening, but the stability is slightly deteriorated after heat storage, the suspension rate is reduced, a small amount of fine powder appears, the wetting time is slow, and the lasting foamability is high; the wettable powders prepared in examples 6 to 13 maintain high suspension rates before and after heat storage, show no fine powder after screening, and have good heat storage stability, relatively short wetting time and relatively low persistent foamability. From this analysis, the adjuvants used in the formulations of examples 6 to 13 can improve the quality of the wettable powder better, and the formulations are more optimized than those of examples 1 to 5. The wettable powder of comparative example 1 has a low suspension rate and a high persistent foamability, and has fine powder before and after heat storage, increased fine powder after heat storage, and poor heat storage stability.

The wettable powder of the topramezone and the cloransulam-methyl prepared in the above examples and comparative examples is quantitatively diluted 1000 times with standard C water, the wettability, the surface tension and the contact angle are detected by a canvas method, and the application indexes are obtained by respectively measuring with a A101Plus type surface tension meter of Shanghai Clematis information technology Co., Ltd and a DSA25 standard type contact angle measuring instrument of Kluyverz science Co., Ltd (Shanghai).

The test results are shown in table 3 below.

TABLE 3 application index conditions of wettable powder standard C water prepared by compounding xaflufen and cloransulam

From the data results in Table 3, it can be seen that the wettable powders of examples 1-5 have a long canvas wetting time of more than 240s, a surface tension of 68 ° or more and a contact angle of more than 70 ° at a chemical solution dilution concentration of 1000 times by quantitative dilution. On the other hand, the wettable powder solutions of examples 6 to 13 have a wetting time of 65 seconds or less, a surface tension of 54 degrees or less, a contact angle of less than 60 degrees, a small contact angle and surface tension value, and a high wettability, and thus it can be seen that the wettable powder solutions of examples 6 to 13 can be well wetted and spread on the surfaces of the weeds, which is advantageous for improving the drug effect.

Test of drug efficacy

The effect of the wettable powder containing the sulfuryl pyraoxystrobin and the cloransulam-methyl for preventing and controlling the annual weeds in the soybean field is evaluated by taking a compound preparation of the sulfuryl pyraoxystrobin and the cloransulam-methyl prepared in part of examples as a research object. The control agent is 40% of sulfonylpyraflufen suspending agent and 84% of cloransulam water dispersible granule (commercially available). The total number of 4 treatments are respectively as follows: treatment 1: spraying clear water, and blank control; and (3) treatment 2: the wettable powder of the sulfonylpyraflufen-cloransulam obtained in part of the examples; and (3) treatment: 40% of a fonflufen suspending agent; and (4) treatment: 84% cloransulam-methyl water dispersible granules.

In the examples, the wettable powder of the sulfonylureas pyraoxystrobin and cloransulam-methyl obtained in the example is subjected to stem leaf spray treatment according to the effective component dosage of 120 g/hectare, the treatment 3 is subjected to stem leaf spray treatment according to the effective component dosage of 250 g/hectare, and the treatment 4 is subjected to stem leaf spray treatment according to the effective component dosage of 35 g/hectare.

Spraying stems and leaves after the first three compound leaves of the soybeans and the hard ryegrass grow, and preventing and killing weeds in soybean fields, wherein the weeds in the soybean fields comprise broadleaf weeds such as dayflower, piemarker, endive and the like, and grassy weeds such as crabgrass, cockspur grass, hard ryegrass and the like. The pesticide is applied for 1 time by a worker-farm-16 knapsack manual sprayer, 750kg of water is added to prepare liquid medicine according to the dosage of the preparation per hectare, and the liquid medicine is uniformly sprayed according to the amount of the liquid medicine in the community. The random block arrangement is adopted, 4 times of repetition are carried out, and the area of a cell is 50m²(5m×10m)。

50 days after the application, the influence of each treatment on the fresh weight control effect of the weeds and the safety of the soybeans is investigated.

The investigation method comprises the following steps: each cell is fixed with 4 points, each point is 0.25m²Investigating the area for non-withered weedsFresh weight and calculating the control effect, the calculation formula is as follows:

control effect (%) - (fresh weight of weeds in blank control area-fresh weight of weeds in treatment area) x 100%/fresh weight of weeds in blank control area

Average control effect is gramineous weed control effect + broadleaf weed control effect/2 (the ryegrass is injected in a single investigation mode, and does not do gramineous weed control effect and average control effect data)

The control results for weeds in soybean fields are shown in table 4 below:

table 4 field efficacy test results of various treatment agents for controlling weeds in soybean fields

The test results in the table 4 show that the compound of the xaflufen and the cloransulam can effectively control annual and perennial weeds in the soybean field, the control effect on annual and perennial grassy and broadleaf weeds in the soybean field 50 days after the application is obviously better than that of 2 control agents, the synergistic effect is shown, and the compound also has good control effect on resistant hard ryegrass. Among them, examples 6, 7, 11, 12, and 13 using the preferred auxiliaries are significantly superior to examples 2, 3, and 5 in effect. According to the observation of the whole field test process, the soybean grows well within the test dosage range, and each treatment agent has no phytotoxicity phenomenon on the soybean, which indicates that the compound preparation is safe to the soybean.

The embodiments show that the wettable powder containing the topramezone and the cloransulam, provided by the invention, has a good synergistic effect, enlarges a weeding spectrum, improves a drug lasting period, delays the generation of drug resistance, and has a good effect of preventing and treating annual and perennial weeds in a soybean field. In addition, the wettable powder product in the embodiment of the invention has simple preparation process and excellent product quality, and is beneficial to application.