Saflufenacil-containing microemulsion as well as preparation method and application thereof

Abstract

The invention relates to the technical field of pesticide microemulsions, in particular to a saflufenacil-containing microemulsion as well as a preparation method and application thereof. The invention relates to a micro-emulsion containing saflufenacil, which is prepared from the following raw materials in percentage by mass: 1 to 5 percent of saflufenacil, 5 to 30 percent of refined glufosinate-ammonium, 2 to 16 percent of solvent, 18 to 32 percent of emulsifier, 0 to 10 percent of cosolvent and the balance of water. The cold storage stability of the microemulsion can be improved by limiting the octyl decyl alcohol polyether phosphate and the tristyrylphenol polyoxyethylene ether ammonium sulfate as the emulsifier. The stability of the microemulsion at low temperature can be improved by limiting the type of the emulsifier and the type of the cosolvent, and the clear and transparent microemulsion is obtained.

Description

Technical Field

[0001] The invention relates to the technical field of pesticide microemulsions, and in particular to a microemulsion containing benzylpyridamole and a preparation method and application thereof. Background Art

[0002] Commonly used herbicides formed by one active herbicidal ingredient have a narrow weed control spectrum, and will increase the resistance of grasses. In addition, the dosage of the herbicide needs to be increased to produce a certain weed control effect, which will lead to the problem of increased use costs and increased environmental pollution. Therefore, it is necessary to develop an environmentally friendly water-based herbicide with a wide weed control spectrum. In order to expand the weed control spectrum, multiple active herbicidal ingredients are currently used in combination to improve the weed control spectrum of the herbicide; for benzaclostrobin, it has excellent control effects on sedge weeds and grass weeds, and can also be used in combination with other herbicides. For glufosinate ammonium, it is a broad-spectrum contact herbicide ingredient with the characteristics of ammonium accumulation and contact killing, and also has good rapidity and a long lasting effect, and has the characteristics of a wider weed control spectrum; however, when benzaclostrobin and glufosinate ammonium preparations are added to water, a high salt system will be formed, which is easy to form unstable thermal motion between ions, thereby affecting the stability of the compounded water-based herbicide.

[0003] A Chinese patent with patent application number CN201910756485.X discloses an emulsifier suitable for glufosinate-ammonium / fluoropyralid microemulsion and an application method thereof, and discloses the use of styrylphenol polyoxyethylene ether, modified alkyl glycoside, alkylphenol polyoxyethylene ether polyoxypropylene ether, and dodecylhydroxysulfobetaine to solve the problems of stratification, crystallization, and precipitation. However, the system cannot solve the problem of stability of the microemulsion forming a high-salt system.

[0004] Therefore, providing a microemulsion containing benzylpyridamole with good stability is the main technical problem that needs to be solved at present. Summary of the invention

[0005] Regarding the stability of the microemulsion containing benzylpyridamole, the microemulsion is currently required to be clear and transparent from the perspective of physical stability. When the particle size of the microemulsion becomes larger, the homogeneous state of the microemulsion will be affected, and a clear and transparent state cannot be obtained, which affects the microemulsion's control effect on weeds. From the perspective of chemical stability, the microemulsion must be able to maintain a decomposition rate of benzylpyridamole of less than or equal to 5% during storage to ensure the microemulsion's control effect on weeds.

[0006] In order to solve the above technical problems, the first aspect of the present invention provides a microemulsion containing benzylpyridinium, and its preparation raw materials include, by mass percentage: 1%-5% benzylpyridinium, 5%-30% glufosinate ammonium, 2%-16% solvent, 18%-32% emulsifier, 0-10% cosolvent, and the balance water.

[0007] In one embodiment, the water is deionized water.

[0008] In one embodiment, the emulsifier includes one or more combinations of phosphate compounds, polyarylphenol polyether compounds, fatty alcohol polyether compounds, polyoxyethylene ether compounds, and alkyl glycoside compounds.

[0009] In one embodiment, the phosphate ester compound includes octanol polyether phosphate, modified phenethylphenol polyoxyethylene ether and its phosphate ester, and a phosphate ester emulsifier.

[0010] In one embodiment, the manufacturer of the octanol polyether phosphate is Beijing Avite Biotechnology Co., Ltd., with the brand name AVT01.

[0011] In one embodiment, the modified phenethylphenol polyoxyethylene ether and phosphate ester thereof can be purchased from Fuzhou Sugest New Material Technology Co., Ltd., with the brand name SG-4001.

[0012] In one embodiment, the phosphate emulsifier can be purchased from Shanghai Xuezhuo Fine Chemical Co., Ltd. under the brand name Featdis TXP.

[0013] In one embodiment, the polyarylphenol polyether compound is composed of polyarylphenol polyether, alkylbenzene sulfonate, and water, and can be purchased from Jiangsu Qingyu Chemical Technology Co., Ltd. with a brand name of SP-ME3625.

[0014] In one embodiment, the fatty alcohol polyether compound includes modified fatty alcohol polyoxyethylene ether-sulfopropionate salt and its derivatives, which can be purchased from Fuzhou Sugest New Material Technology Co., Ltd. with a brand name of SG-2003.

[0015] Polyoxyethylene ether compound (AVT-02 (tristyrylphenol polyoxyethylene ether ammonium sulfate)).

[0016] In one embodiment, the polyoxyethylene ether compound includes tristyrylphenol polyoxyethylene ether ammonium sulfate.

[0017] In one embodiment, the tristyrylphenol polyoxyethylene ether ammonium sulfate salt can be purchased from Beijing Avite Biotechnology Co., Ltd. with the brand name AVT-02.

[0018] In one embodiment, the alkyl glycoside can be purchased from Shanghai Xuezhuo Fine Chemical Co., Ltd. under the brand name Featwet 1009.

[0019] The alkyl glycoside compound formed by the composition consisting of alkyl glycoside, polyarylphenol polyether, alkylbenzene sulfonate and water can be purchased from Jiangsu Qingyu Chemical Technology Co., Ltd., with the brand name SP-ME3639.

[0020] In one embodiment, the emulsifier includes a phosphate compound and a polyoxyethylene ether compound, and the mass ratio of the phosphate compound to the polyoxyethylene ether compound is (1-2): (0.5-2).

[0021] In one embodiment, the mass ratio of the phosphate compound to the polyoxyethylene ether compound in the emulsifier is (1-1.6): (0.6-1.4).

[0022] In order to improve the stability of the microemulsion containing benzylpyridinium chloride, especially the stability at low temperature, the inventors found that the use of a specific emulsifier, especially octyl decyl alcohol polyether phosphate and tristyrylphenol polyoxyethylene ether ammonium sulfate as an emulsifier, when the mass ratio of the octyl decyl alcohol polyether phosphate and the tristyrylphenol polyoxyethylene ether ammonium sulfate is 1:1.25, and the microemulsion obtained by using the emulsifier in combination with a cosolvent formed by any one of ethanol, n-butanol, ethylene glycol, propylene glycol, glycerol, and isopropanol can improve the stability of the microemulsion at low temperature and obtain a clear and transparent microemulsion.

[0023] In order to improve the stability of the microemulsion containing benzylpyridinium, especially the stability at low temperature, the inventors found that when a specific emulsifier is used and no co-solvent is added, octanol polyether phosphate and tristyrylphenol polyoxyethylene ether ammonium sulfate are limited as emulsifiers, the mass ratio of octanol polyether phosphate and tristyrylphenol polyoxyethylene ether ammonium sulfate is limited to 1.4:1, and the mass proportion of the emulsifier is limited to 24%, the cold storage stability of the microemulsion can be improved; the mass ratio of octanol polyether phosphate and tristyrylphenol polyoxyethylene ether ammonium sulfate is limited to 1.6:1.4, and the mass proportion of the emulsifier is 30%, the cold storage stability of the microemulsion can be improved.

[0024] In order to improve the stability of the microemulsion containing benzylpyridinium, especially the stability at low temperature, the inventors found that when a specific emulsifier and a cosolvent are used in combination, octanol polyether phosphate and tristyrylphenol polyoxyethylene ether ammonium sulfate are limited as emulsifiers, the mass ratio of octanol polyether phosphate and tristyrylphenol polyoxyethylene ether ammonium sulfate is limited to 1.4:0.6, and the mass proportion of the emulsifier is limited to 20%. When the microemulsion is used in combination with a cosolvent formed by any one of ethanol, ethylene glycol, and isopropanol, the stability of the microemulsion at low temperature can be improved to obtain a clear and transparent microemulsion.

[0025] In one embodiment, the emulsifier comprises an alkyl glycoside compound and a polyarylphenol polyether compound, and the mass ratio of the alkyl glycoside compound to the polyarylphenol polyether compound is (2-3): (0.5-1.5).

[0026] In a preferred embodiment, the mass ratio of the alkyl glycoside compound to the polyarylphenol polyether compound in the emulsifier is (2-2.75): (0.6-1).

[0027] In a preferred embodiment, the mass ratio of the alkyl glycoside compound to the polyarylphenol polyether compound is (2-2.4): (0.6-0.8).

[0028] In order to improve the stability of the microemulsion containing benzylpyridinium, especially the stability at low temperature, keep the decomposition rate of benzylpyridinium less than or equal to 5%, obtain qualified products, and ensure the control effect of the microemulsion on weeds; the inventors found in the experiment that the emulsifier used in the microemulsion is composed of alkyl glycoside compounds and polyarylphenol polyether compounds, and when the mass proportion of the emulsifier in the preparation raw materials of the microemulsion is 26-32%, the mass proportion of the alkyl glycoside compounds is 20-24%, and the mass ratio of the alkyl glycoside compounds to the polyarylphenol polyether compounds is (2-3): (0.5-1.5), preferably The mass ratio of the alkyl glycoside compound to the polyarylphenol polyether compound in the emulsifier is selected to be (2-2.75): (0.6-1), and more preferably the mass ratio of the alkyl glycoside compound to the polyarylphenol polyether compound is (2-2.4): (0.6-0.8). The microemulsion formed by the coordinated action of the solvent and the co-solvent with benzylpyridazine and glufosinate-ammonium can maintain the pH of the microemulsion at 4-5, which can not only improve the storage stability of the microemulsion at low temperature, but also keep the decomposition rate of benzylpyridazine less than or equal to 5%, thereby obtaining a qualified product and ensuring the control effect of the microemulsion on weeds.

[0029] In order to improve the stability of the microemulsion containing benzylpyridinium, especially the stability at low temperature, the inventors found in the experimental process that when no co-solvent is added to the microemulsion, a clear and transparent microemulsion cannot be obtained at room temperature and under cold storage conditions. When a co-solvent is added to the microemulsion, the co-solvent added in an amount of 4% and used in combination with an alkyl glycoside compound (emulsifier SP-ME3639) and a polyarylphenol polyether compound (emulsifier SP-ME3625) cannot effectively improve the state of the microemulsion at room temperature and under cold storage conditions, and a clear and transparent microemulsion cannot be obtained; when the co-solvent addition amount is limited to 6-10%, and the co-solvent is limited to any one of ethanol, propylene glycol, glycerol, and isopropanol, the state of the microemulsion at room temperature and under cold storage conditions can be effectively improved, and a clear and transparent microemulsion can be obtained.

[0030] In a preferred embodiment, the mass ratio of the alkyl glycoside compound to the polyarylphenol polyether compound is 2.75:1.

[0031] The inventors found during the experiment that when the solvent is limited to 150# solvent oil or dimethyl octanamide, the mass ratio of the solvent to benzaclostrobin is (2-6):1, the mass proportion of the solvent is 2-6%, and the emulsifier is limited to be composed of an alkyl glycoside compound and a polyarylphenol polyether compound, and the mass ratio of the alkyl glycoside compound to the polyarylphenol polyether compound is 2.75:1, the storage stability of the microemulsion at low and high temperatures can be improved. The possible reason is that the solvent in the microemulsion forms an oil phase with the active ingredients benzaclostrobin and glufosinate in the system. When the amount of solvent is increased, the volume of the oil phase increases accordingly, the amount of water is reduced, the number of hydrogen bonds generated in the system is small, the cloud point is lowered, and the stability of the microemulsion is affected.

[0032] In one embodiment, the solvent includes a combination of one or more of xylene, solvent oil, and dimethyl octanamide.

[0033] In one embodiment, the solvent oil is 150# solvent oil.

[0034] In one embodiment, the co-solvent includes a combination of one or more of ethanol, n-butanol, ethylene glycol, propylene glycol, glycerol, and isopropanol.

[0035] In one embodiment, the preparation raw material further includes a stabilizer.

[0036] In one embodiment, the preparation raw materials include, by mass percentage, 1%-4% of benzylpyridamole, 5%-12% of glufosinate ammonium, 2%-16% of solvent, 18%-32% of emulsifier, 0-10% of cosolvent, 0.01-1% of stabilizer, and the balance of water.

[0037] The emulsifier is a combination of an alkyl glycoside compound and a polyarylphenol polyether compound.

[0038] In one embodiment, the type of the stabilizer is not limited, and the purpose of adding the stabilizer is to adjust the pH of the microemulsion to 4-5; as experimental cases, the stabilizer can be selected from citric acid, potassium dihydrogen phosphate, and lactic acid.

[0039] In one embodiment, the pH of the microemulsion containing benzylpyridamole is 4-5.

[0040] The inventors found during the experiment that the chemical stability also needs to be considered when the microemulsion maintains good physical stability. After storage at high temperature, the decomposition rate of benzylpyridazine needs to be controlled. In order to solve the problem that the decomposition rate of benzylpyridazine can be kept less than or equal to 5% during the storage of the microemulsion, the inventors found during the experiment that the pH of the microemulsion is limited to 4-5, and phosphate compounds and polyoxyethylene ether compounds are used as emulsifiers or alkyl glycoside compounds and polyarylphenol polyether compounds are used as emulsifiers to cooperate with specific solvents and specific co-solvents. The chemical stability of the microemulsion can be improved, and the decomposition rate of benzylpyridazine can be kept less than or equal to 5% during the storage process; the possible reason is that limiting the pH of the microemulsion can not only maintain the homogeneous state of the microemulsion, but also reduce the risk of ester bond breakage in benzylpyridazine, thereby maintaining the decomposition rate of benzylpyridazine less than or equal to 5%, obtaining qualified products, and ensuring the weed control effect of the microemulsion.

[0041] The second aspect of the present invention provides a method for preparing a microemulsion containing benzylpyridamole, comprising the following steps:

[0042] S1. adding fenthion to a solvent to dissolve it, and then adding an emulsifier to mix well to obtain a mixture a;

[0043] S2. The refined glufosinate was added to water, and then the co-solvent was added to the water and mixed to obtain a mixture b;

[0044] S3. Add mixture a into mixture b and mix them evenly to obtain a microemulsion.

[0045] In one embodiment, the method for preparing the microemulsion containing benzylpyridamole comprises the following steps:

[0046] S1. adding fenthion to a solvent to dissolve it, and then adding an emulsifier to mix well to obtain a mixture a;

[0047] S2. The refined glufosinate is added to water, and then a cosolvent and a stabilizer are added to the water and mixed to obtain a mixture b;

[0048] S3. Add mixture a into mixture b and mix them evenly to obtain a microemulsion.

[0049] The third aspect of the present invention provides an application of a microemulsion containing benzaclostrobin, wherein the microemulsion containing benzaclostrobin is applied in the technical field of weed control.

[0050] Beneficial Effects

[0051] 1. In the present invention, the cold storage stability of the microemulsion can be improved by limiting octyl decyl alcohol polyether phosphate and tristyrylphenol polyoxyethylene ether sulfate ammonium salt as emulsifiers, and the pH of the microemulsion is adjusted to 4-5 after adding a stabilizer, so that the decomposition rate of benzylpyraclostrobin can be kept less than or equal to 5%, thereby obtaining a qualified product and ensuring the control effect of the microemulsion on weeds.

[0052] 2. In the present invention, by limiting the type of emulsifier and the type of cosolvent, the stability of the microemulsion at low temperature can be improved to obtain a clear and transparent microemulsion.

[0053] 3. In the present invention, by limiting the emulsifier to consist of alkyl glycoside compounds and polyaromatic phenol polyether compounds, the mass proportion of the emulsifier in the preparation raw materials of the microemulsion is 26-32%, the mass proportion of the alkyl glycoside compounds is 20-24%, and the microemulsion formed by the coordinated action of the solvent and the co-solvent with benzylpyridazine and glufosinate-ammonium can improve the storage stability of the microemulsion at low temperatures, make the pH of the microemulsion 4-5, keep the decomposition rate of benzylpyridazine less than or equal to 5%, obtain qualified products, and ensure the control effect of the microemulsion on weeds.

[0054] 4. In the present invention, no cosolvent is added, and the use of a specific emulsifier can improve the stability of the microemulsion containing benzylpyridamole, especially the stability at low temperature.

[0055] 5. In the present invention, when the solvent is limited to 150# solvent oil or dimethyl octanamide, the mass ratio of the solvent to benzylpyrazoline is (2-6):1, the mass proportion of the solvent is 2-6%, and when the emulsifier is limited to be composed of alkyl glycoside compounds and polyarylphenol polyether compounds, the storage stability of the microemulsion at low and high temperatures can be improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0056] The stability test of the microemulsion containing benzylpyridamole provided in Examples 1 to 47 was carried out. The test results showed different microemulsion states. The specific states are shown in Figure 1-7 .

[0057] Figure 1 Provides clarity and transparency in test results.

[0058] Figure 2 The result is opaque and contains precipitates.

[0059] Figure 3 There is an oily precipitate at the bottom.

[0060] Figure 4 To clarify transparent and opaque states.

[0061] Figure 5The serial number 1 represents the pure milky white state, the serial number 2 represents the fuzzy opaque state, the serial number 3 represents the fuzzy opaque state, and the serial number 4 represents the translucent state.

[0062] Figure 6 It is the state where there is white sediment at the bottom of the test result.

[0063] Figure 7 It is the state in which there is an incompletely emulsified layer on the top of the microemulsion in the test results.

[0064] Figure 8 This is the effect of the blank control, and no herbicide was applied to Goosegrass.

[0065] Fig. 9 The herbicide containing only 1% of benzylpyridamole as the active ingredient has a herbicidal effect on goosegrass after application.

[0066] Fig.10 The herbicide containing only 10% glufosinate as the active ingredient has a herbicide that has a herbicidal effect on goosegrass after application.

[0067] Fig.11 This is the herbicidal effect of a microemulsion containing 1% benzylpyridamole and 10% glufosinate (used at a dosage of 200 mL / mu) on goosegrass.

[0068] Fig.12 The herbicidal effect of the microemulsion containing 1% benzylpyridamole and 10% glufosinate provided in Example 11 (used in an amount of 150 mL / mu) on goosegrass after application. DETAILED DESCRIPTION

[0069] The sources of raw materials used in the following experiments are shown in Table y-1.

[0070] Table y-1

[0071]

[0072] The purity of the benzylpyridamole used in the following examples is 95%.

[0073] The purity of the refined glufosinate-ammonium used in the examples is 90%.

[0074] The first group of experiments provided a microemulsion containing benzylpyridamole, the preparation raw materials of which included benzylpyridamole, glufosinate ammonium, solvent, emulsifier, cosolvent and water. The specific addition amounts of the raw materials were shown in Table 1-1 in terms of mass percentage.

[0075] The water is deionized water.

[0076] The solvent is xylene.

[0077] The emulsifier consists of octanol polyether phosphate and tristyrylphenol polyoxyethylene ether ammonium sulfate.

[0078] The co-solvent is any one of ethanol, n-butanol, ethylene glycol, glycerol and isopropanol.

[0079] The manufacturer of the octanol polyether phosphate is Beijing Avite Biotechnology Co., Ltd., and the brand is AVT-01. The brand is used instead of the raw material name of the emulsifier in Table 1-1.

[0080] The tristyrylphenol polyoxyethylene ether ammonium sulfate salt was purchased from Beijing Avite Biotechnology Co., Ltd., with the brand name AVT-02. The brand name is used instead of the raw material name of the emulsifier in Table 1-1.

[0081] The first group of experiments provides a method for preparing a microemulsion containing benzylpyridamole, comprising the following steps:

[0082] S1. adding fenthion to a solvent to dissolve it, and then adding an emulsifier to mix well to obtain a mixture a;

[0083] S2. The refined glufosinate was added to water, and then the co-solvent was added to the water and mixed to obtain a mixture b;

[0084] S3. Add mixture a into mixture b and mix them evenly to obtain a microemulsion.

[0085] The first group of experiments provides an application of a microemulsion containing benzaclostrobin, wherein the microemulsion containing benzaclostrobin is applied in the technical field of weed control.

[0086] Table 1-1

[0087]

[0088]

[0089] The second group of experiments provided a microemulsion containing benzylpyridamole, the raw materials for its preparation included: benzylpyridamole, glufosinate ammonium, solvent, emulsifier, and water. The specific addition amounts of the raw materials, calculated by mass percentage, are shown in Table 1-2.

[0090] The preparation raw materials also include a co-solvent, and the specific amount added is shown in Table 1-2.

[0091] The solvent is xylene.

[0092] The water is deionized water.

[0093] The emulsifier consists of octanol polyether phosphate and tristyrylphenol polyoxyethylene ether ammonium sulfate.

[0094] The co-solvent is any one of ethanol, ethylene glycol and isopropanol.

[0095] The manufacturer of the octanol polyether phosphate is Beijing Avite Biotechnology Co., Ltd., and the brand is AVT-01. In Table 1-2, the brand is used instead of the raw material name of the emulsifier.

[0096] The tristyrylphenol polyoxyethylene ether ammonium sulfate salt was purchased from Beijing Avite Biotechnology Co., Ltd., with the brand name AVT-02. The brand name is used instead of the raw material name of the emulsifier in Table 1-2.

[0097] The second group of experiments provided a preparation method of a microemulsion containing benzylpyridamole, which was the same as that in Example 1. For the example in which no co-solvent was added, the step of adding the co-solvent was omitted in the preparation method.

[0098] The second group of experiments provided the same application of the microemulsion containing benzylpyridamole as in Example 1.

[0099] Table 1-2

[0100]

[0101]

[0102] The third group of experiments provided a microemulsion containing benzylpyridamole, the raw materials for its preparation included: benzylpyridamole, glufosinate ammonium, solvent, emulsifier, cosolvent, and water. The specific addition amounts of the raw materials, calculated by mass percentage, are shown in Tables 1-3.

[0103] The water is deionized water.

[0104] The solvent is 150# solvent oil.

[0105] The cosolvent is ethanol.

[0106] The emulsifier consists of alkyl glycoside compounds and polyarylphenol polyether compounds.

[0107] The alkyl glycoside compound is a composition consisting of alkyl glycoside, polyarylphenol polyether, alkylbenzene sulfonate and water. It is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd. and has a brand name of SP-ME3639. The brand name is used instead of the raw material name of the emulsifier in Tables 1-3.

[0108] The polyarylphenol polyether compound is a composition consisting of polyarylphenol polyether, alkylbenzene sulfonate, methanol and water. It is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd. and has a brand name of SP-ME3625. The brand name is used instead of the raw material name of the emulsifier in Tables 1-3.

[0109] The third group of experiments provided a method for preparing a microemulsion containing benzylpyridamole, which was the same as that in Example 1.

[0110] The third group of experiments provided the same application of the microemulsion containing benzylpyridamole as in Example 1.

[0111] Table 1-3

[0112]

[0113] The fourth group of experiments provided a microemulsion containing benzaclostrobin, the raw materials for its preparation included: benzaclostrobin, glufosinate ammonium, solvent, emulsifier, cosolvent, water, and the specific addition amounts of the raw materials were shown in Tables 1-4 in terms of mass percentage.

[0114] The water is deionized water.

[0115] The solvent is dimethyl octanamide.

[0116] The cosolvent is ethanol.

[0117] The emulsifier consists of alkyl glycoside compounds and polyarylphenol polyether compounds.

[0118] The alkyl glycoside compound is a composition consisting of alkyl glycoside, polyarylphenol polyether, alkylbenzene sulfonate and water. The manufacturer is Jiangsu Qingyu Chemical Technology Co., Ltd., and the brand is SP-ME3639. The brand is used instead of the raw material name of the emulsifier in Tables 1-4.

[0119] The polyarylphenol polyether compound is a composition consisting of polyarylphenol polyether, alkylbenzene sulfonate, methanol and water. It is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd. and has a brand name of SP-ME3625. The brand name is used instead of the raw material name of the emulsifier in Tables 1-4.

[0120] The fourth group of experiments provided a method for preparing a microemulsion containing benzylpyridamole, which was the same as that in Example 1.

[0121] The fourth group of experiments provided the same application of the microemulsion containing benzylpyridamole as in Example 1.

[0122] Table 1-4

[0123]

[0124]

[0125] The fifth group of experiments provided a microemulsion containing benzaclostrobin, the raw materials for its preparation included: benzaclostrobin, glufosinate ammonium, solvent, emulsifier, cosolvent, and water. The specific addition amounts of the raw materials, calculated by mass percentage, are shown in Tables 1-5.

[0126] The water is deionized water.

[0127] The solvent is 150# solvent oil.

[0128] The cosolvent is ethanol.

[0129] The emulsifier consists of alkyl glycoside compounds and polyarylphenol polyether compounds.

[0130] The alkyl glycoside compound is a composition consisting of alkyl glycoside, polyarylphenol polyether, alkylbenzene sulfonate and water. The manufacturer is Jiangsu Qingyu Chemical Technology Co., Ltd., and the brand is SP-ME3639. The brand is used instead of the raw material name of the emulsifier in Tables 1-5.

[0131] The polyarylphenol polyether compound is a composition consisting of polyarylphenol polyether, alkylbenzene sulfonate, methanol and water. It is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd. and has a brand name of SP-ME3625. The brand name is used instead of the raw material name of the emulsifier in Tables 1-5.

[0132] The fifth group of experiments provided a method for preparing a microemulsion containing benzylpyridamole, which is the same as that in Example 1.

[0133] The fifth group of experiments provided the same application of the microemulsion containing benzylpyridamole as in Example 1.

[0134] Table 1-5

[0135]

[0136]

[0137] The sixth group of experiments provided a microemulsion containing benzaclostrobin, the raw materials for its preparation included: benzaclostrobin, glufosinate ammonium, solvent, emulsifier, cosolvent, and water. The specific addition amounts of the raw materials, calculated by mass percentage, are shown in Table 1-6.

[0138] The water is deionized water.

[0139] The solvent is 150# solvent oil.

[0140] The cosolvent is ethanol.

[0141] The emulsifier consists of alkyl glycoside compounds and polyarylphenol polyether compounds.

[0142] The alkyl glycoside compound is a composition consisting of alkyl glycoside, polyarylphenol polyether, alkylbenzene sulfonate and water. It is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd. and has a brand name of SP-ME3639. The brand name is used instead of the raw material name of the emulsifier in Tables 1-6.

[0143] The polyarylphenol polyether compound is a composition consisting of polyarylphenol polyether, alkylbenzene sulfonate, methanol and water. It is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd. and has a brand name of SP-ME3625. The brand name is used instead of the raw material name of the emulsifier in Tables 1-6.

[0144] The sixth group of experiments provided a method for preparing a microemulsion containing benzylpyridamole, which was the same as that in Example 1.

[0145] The sixth group of experiments provided the same application of the microemulsion containing benzylpyridamole as in Example 1.

[0146] Table 1-6

[0147]

[0148] The seventh group of experiments provided a microemulsion containing benzaclostrobin, the raw materials for its preparation included: benzaclostrobin, glufosinate ammonium, solvent, emulsifier, cosolvent, stabilizer, and water. The specific addition amounts of the raw materials, calculated by mass percentage, are shown in Tables 1-7.

[0149] The water is deionized water.

[0150] The solvent is 150# solvent oil.

[0151] The cosolvent is ethanol.

[0152] The stabilizer is citric acid.

[0153] The emulsifier consists of alkyl glycoside compounds and polyarylphenol polyether compounds.

[0154] The alkyl glycoside compound is a composition consisting of alkyl glycoside, polyarylphenol polyether, alkylbenzene sulfonate and water. The manufacturer is Jiangsu Qingyu Chemical Technology Co., Ltd., and the brand is SP-ME3639. The brand is used instead of the raw material name of the emulsifier in Tables 1-5.

[0155] The polyarylphenol polyether compound is a composition consisting of polyarylphenol polyether, alkylbenzene sulfonate, methanol and water. It is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd. and has a brand name of SP-ME3625. The brand name is used instead of the raw material name of the emulsifier in Tables 1-5.

[0156] The seventh group of experiments provides a method for preparing a microemulsion containing benzylpyridamole, comprising the following steps:

[0157] S1. adding fenthion to a solvent to dissolve it, and then adding an emulsifier to mix well to obtain a mixture a;

[0158] S2. The refined glufosinate is added to water, and then a cosolvent and a stabilizer are added to the water and mixed to obtain a mixture b;

[0159] S3. Add mixture a into mixture b and mix them evenly to obtain a microemulsion.

[0160] The seventh group of experiments provided the same application of the microemulsion containing benzylpyridamole as in Example 1.

[0161] Table 1-7

[0162]

[0163] The eighth group of experiments provides a microemulsion containing benzaclostrobin, the raw materials for its preparation include: benzaclostrobin, glufosinate-ammonium, solvent, emulsifier, cosolvent, stabilizer, water, and the specific addition amounts of the raw materials are shown in Tables 1-8 by mass percentage. Tables 1-8 provide Examples 59, 60, 61, 62, and 63.

[0164] The water is deionized water.

[0165] The stabilizer is citric acid.

[0166] The emulsifier consists of alkyl glycoside compounds and polyarylphenol polyether compounds.

[0167] The alkyl glycoside compound is a composition consisting of alkyl glycoside, polyarylphenol polyether, alkylbenzene sulfonate and water. The manufacturer is Jiangsu Qingyu Chemical Technology Co., Ltd., and the brand is SP-ME3639. The brand is used instead of the raw material name of the emulsifier in Tables 1-5.

[0168] The polyarylphenol polyether compound is a composition consisting of polyarylphenol polyether, alkylbenzene sulfonate, methanol and water. It is purchased from Jiangsu Qingyu Chemical Technology Co., Ltd. and has a brand name of SP-ME3625. The brand name is used instead of the raw material name of the emulsifier in Tables 1-5.

[0169] The solvent used in Example 59 and Example 60 is dimethyl octanamide, and the co-solvent used is ethanol.

[0170] The solvent used in Example 61, Example 62, and Example 63 is 150# solvent oil.

[0171] The co-solvent used in Example 61 is ethanol.

[0172] The co-solvent used in Example 62 is propylene glycol.

[0173] The co-solvent used in Example 63 is propylene glycol.

[0174] The preparation method of the microemulsion containing benzylpyridamole provided by the eighth group of experiments is the same as that of the seventh group of experiments.

[0175] S1. adding fenthion to a solvent to dissolve it, and then adding an emulsifier to mix well to obtain a mixture a;

[0176] S2. The refined glufosinate is added to water, and then a cosolvent and a stabilizer are added to the water and mixed to obtain a mixture b;

[0177] S3. Add mixture a into mixture b and mix them evenly to obtain a microemulsion.

[0178] The eighth group of experiments provided the same application of the microemulsion containing benzylpyridamole as in Example 1.

[0179] Table 1-8

[0180]

[0181]

[0182] Performance Testing

[0183] 1. Stability test:

[0184] The microemulsions containing benzylpyridamole provided in Examples 1 to 47 were tested for microemulsion stability, low temperature stability, and thermal storage stability according to the test methods provided in Table a-1. The test results are shown in Tables 2-1, 2-2, 2-3, 2-4, 2-5, 2-6, 2-7, and 2-8.

[0185] 2. Application of herbicidal effect test:

[0186] (1) Test on the weed control effect of Goosegrass:

[0187] Application location: Nantong, Jiangsu;

[0188] Weed Type: Goosegrass;

[0189] Apply to Goosegrass separately:

[0190] ① The herbicide containing only 1% of the active ingredient benzylpyridamole (the dosage is 40mL / mu), the effect is seen after 7 days of application Fig. 9 .

[0191] ② The herbicide containing only 10% glufosinate as the active ingredient (the dosage is 200mL / mu), the effect is seen after 7 days of application Fig.10 .

[0192] ③ The stability test in the third to sixth experiments verified that the microemulsion containing 1% benzylpyrazone and 10% glufosinate ammonium (the dosage was 200mL / mu) with a clear and transparent effect was effective after 7 days of application. Fig.11 .

[0193] ④ The stability test was carried out in the third to sixth experiments to verify the effect of the clear and transparent microemulsion containing 1% benzylpyridazine and 10% glufosinate (dosage is 150mL / mu). The effect was seen after 7 days of application. Fig.12 .

[0194] Figure 8 As a blank control effect, no herbicide was applied to Goosegrass.

[0195] pass Figure 1-4 It can be seen that when using only the herbicide containing benzylpyridazine and the herbicide containing glufosinate, the goosegrass was not completely killed after 7 days of application; but after using the microemulsion containing 1% benzylpyridazine and 10% glufosinate, the density of the treated goosegrass was higher, the goosegrass was completely killed, and the synergistic effect was obvious. Figure 5 It can be seen that when the dosage of the microemulsion containing 1% benzylpyridamole and 10% glufosinate was reduced to 150 mL / mu, the control effect on goosegrass was stable and the goosegrass died completely.

[0196] 3. pH test:

[0197] Test method: Referring to GB T 1601-1993 Standard for the determination of pH value of pesticides, the microemulsion containing benzylpyridamole was diluted 100 times with deionized water and its pH was tested.

[0198] The pH of the microemulsions containing benzylpyridamole provided in Examples 1-6 was tested, and the test results are shown in Table 2-1.

[0199] The pH of the microemulsions containing benzylpyridamole provided in Examples 7-19 was tested, and the test results are shown in Table 2-2.

[0200] The pH of the microemulsions containing benzylpyridamole provided in Examples 48-58 were tested, and the test results are shown in Tables 2-7.

[0201] The pH of the microemulsions containing benzylpyridamole provided in Examples 59-63 were tested, and the test results are shown in Tables 2-8.

[0202] 4. Test of the decomposition rate of benzothiazide:

[0203] The decomposition rate of benzaclostrobin in the microemulsion containing benzaclostrobin provided in Example 1-6 after heat storage for 14 days was tested. The test results are shown in Table 2-1.

[0204] The decomposition rate of benzaclostrobin in the microemulsion containing benzaclostrobin provided in Example 7-19 after heat storage for 14 days was tested. The test results are shown in Table 2-2.

[0205] The decomposition rate of benzaclostrobin in the microemulsions containing benzaclostrobin provided in Examples 40-42 after 14 days of heat storage was tested. The test results are shown in Tables 2-6.

[0206] The decomposition rate of benzaclostrobin in the microemulsions containing benzaclostrobin provided in Examples 48-58 after heat storage for 14 days was tested. The test results are shown in Tables 2-7.

[0207] The decomposition rate of benzaclostrobin in the microemulsions containing benzaclostrobin provided in Examples 59-63 after heat storage for 14 days was tested. The test results are shown in Tables 2-8.

[0208] The decomposition rate of fenpyroxil (%) = (1-the content of fenpyroxil after hot storage / the content of fenpyroxil in normal storage) * 100%.

[0209] Table a-1

[0210]

[0211] Table 2-1

[0212]

[0213]

[0214] By observing the fresh preparation, cold storage and hot storage stability of the microemulsion containing benzylpyridamole provided in the examples of the first group of experiments, the experimental results in Table 2-1 were obtained. From the experimental results in Table 2-1, it can be seen that the addition of specific co-solvents (ethanol, n-butanol, ethylene glycol, glycerol, isopropanol) can improve the stability of the microemulsion at low temperatures.

[0215] Table 2-2

[0216]

[0217] By preparing the microemulsion containing benzylpyridinium provided in the second group of experimental examples and observing the cold storage and hot storage stability, the experimental results in Table 2-2 were obtained. The experimental results in Table 2-2 show that selecting a specific type of emulsifier in this patent can improve the cold storage stability of the microemulsion. When the emulsifier octanol polyether phosphate and the emulsifier tristyrylphenol polyoxyethylene ether ammonium sulfate are limited to a mixing ratio of 1.4:1, so that the mass proportion of the emulsifier is 24%, the cold storage stability of the microemulsion can be improved; when the mass ratio of the emulsifier octanol polyether phosphate and the emulsifier tristyrylphenol polyoxyethylene ether ammonium sulfate is limited to 1.6:1.4, the cold storage stability of the microemulsion can be improved when the mass ratio of the emulsifier is 30%; when the mass ratio of the emulsifier octanol polyether phosphate and the emulsifier tristyrylphenol polyoxyethylene ether ammonium sulfate is limited to 1.4:0.6, the cold storage stability of the microemulsion can be improved when the mass ratio of the emulsifier is 20%.

[0218] Table 2-3

[0219]

[0220] Table 2-4

[0221]

[0222] From the stability test results of the microemulsion containing benzylpyridazine provided by the third and fourth experiments, it can be seen that the mass ratio of the solvent to benzylpyridazine is (2-6):1, and when the solvent is 150# solvent oil or dimethyl octanamide, the storage stability of the microemulsion at low and high temperatures can be improved.

[0223] Table 2-5

[0224]

[0225] From the stability test results of the microemulsion containing benzylpyridamole provided by the fifth group of experiments, it can be seen that the emulsifier used in the microemulsion is composed of alkyl glycoside compounds and polyarylphenol polyether compounds. When the mass proportion of the emulsifier in the preparation raw materials of the microemulsion is 26-32% and the mass proportion of the alkyl glycoside compounds is 20-24%, the storage stability of the microemulsion at low temperatures can be improved.

[0226] Table 2-6

[0227]

[0228]

[0229] From the stability test results of the microemulsion containing benzylpyridinium provided by the sixth group of experiments, it can be seen that when no co-solvent is added to the microemulsion, a clear and transparent microemulsion cannot be obtained at room temperature and cold storage conditions. When a co-solvent is added to the microemulsion, the addition of the co-solvent accounts for 4%, and the use of the co-solvent in combination with the emulsifier SP-ME3639 and the emulsifier SP-ME3625 cannot effectively improve the state of the microemulsion at room temperature and cold storage conditions, and a clear and transparent microemulsion cannot be obtained; when the addition amount of the co-solvent is limited to 6-10%, and the co-solvent is limited to any one of ethanol, propylene glycol, glycerol, and isopropanol, the state of the microemulsion at room temperature and cold storage conditions can be effectively improved, and a clear and transparent microemulsion can be obtained, but the decomposition rate of benzylpyridinium is greater than 5%, and the decomposition rate of benzylpyridinium cannot be effectively controlled to be less than or equal to 5%.

[0230] Table 2-7

[0231]

[0232] It can be seen from Table 2-7 that after adding the stabilizer in the seventh group of experiments, the pH of the microemulsion can be maintained at 4-5, and the decomposition rate of benzylpyridamole can be maintained at less than 5%.

[0233] Table 2-8

[0234]

[0235]

[0236] It can be seen from Table 2-8 that after adding the stabilizer in the eighth group of experiments, the pH of the microemulsion can be maintained at 4-5, and the decomposition rate of benzylpyridamole can be maintained at less than 5%.

[0237] The above test results are clear and transparent. Figure 1 ; The opaque and precipitated state in the test results is shown in Figure 2 ; The state of oily precipitate at the bottom of the test results is shown in Figure 3 ; See the test results for clear and opaque states. Figure 4 ; The pure milky white state in the test results is shown in Figure 5 No. 1; the test results are blurred and opaque. Figure 5 No. 2; the test results are blurred and opaque. Figure 5 No. 3; see the semi-transparent state in the test results Figure 5 No. 4; the test results show that there is white sediment at the bottom. Figure 6 In the test results, there is an incompletely emulsified layer on the top of the microemulsion. Figure 7 .

Claims

1. A microemulsion containing benzylpyridamole, characterized in that: Calculated by mass percentage, the preparation raw materials include: 1%-5% of benzylpyrazone, 5%-30% of glufosinate ammonium, 2%-16% of solvent, 18%-32% of emulsifier, 0-10% of co-solvent and the balance of water.

2. The microemulsion containing benzylpyridamole according to claim 1, characterized in that: The emulsifier includes one or more combinations of phosphate compounds, polyarylphenol polyether compounds, fatty alcohol polyether compounds, polyoxyethylene ether compounds, and alkyl glycoside compounds.

3. The microemulsion containing benzylpyridamole according to claim 2, characterized in that: The emulsifier comprises a phosphate compound and a polyoxyethylene ether compound, and the mass ratio of the phosphate compound to the polyoxyethylene ether compound is (1-2): (0.5-2).

4. The microemulsion containing benzylpyridamole according to claim 2, characterized in that: The emulsifier comprises an alkyl glycoside compound and a polyaryl phenol polyether compound, and the mass ratio of the alkyl glycoside compound to the polyaryl phenol polyether compound is (2-3): (0.5-1.5).

5. The microemulsion containing benzylpyridamole according to claim 1, characterized in that: The solvent includes one or more combinations of xylene, solvent oil, and dimethyl octanamide.

6. The microemulsion containing benzylpyridamole according to claim 1, characterized in that: The co-solvent includes one or more combinations of ethanol, n-butanol, ethylene glycol, propylene glycol, glycerol, and isopropanol.

7. The microemulsion containing benzylpyridamole according to claim 1, characterized in that: The preparation raw materials also include a stabilizer.

8. The microemulsion containing benzylpyridamole according to any one of claims 1 to 7, characterized in that: The pH of the microemulsion containing benzylpyridamole is 4-5.

9. A method for preparing a microemulsion containing benzylpyridamole as claimed in claim 1, characterized in that: The following steps are involved: S1. adding fenthion to a solvent to dissolve it, and then adding an emulsifier to mix well to obtain a mixture a; S2. The refined glufosinate was added to water, and then the co-solvent was added to the water and mixed to obtain a mixture b; S3. Add mixture a into mixture b and mix them evenly to obtain a microemulsion.

10. A use of a microemulsion containing benzylpyridamole as claimed in any one of claims 1 to 8, characterized in that: The microemulsion containing benzylpyridamole is applied in the technical field of weed control.

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