Saflufenacil-containing emulsion in water and preparation method thereof

Abstract

The invention relates to the technical field of emulsion in water, in particular to a saflufenacil-containing emulsion in water and a preparation method thereof. The saflufenacil suspending agent is prepared from the following raw materials in percentage by mass: 5-30% of saflufenacil, 10-40% of a solvent, 3-5% of an emulsifier, 3-5% of an anti-freezing agent, 0.01-0.1% of a defoaming agent, 0.1-1% of a stabilizer and the balance of water. The water emulsion containing the saflufenacil provided by the invention has good high-temperature storage stability, the decomposition rate of the saflufenacil is less than 5%, and the shelf life of 2 years is met; the dispersing and diluting properties in water with different hardness are good; the anti-flying agent is simply mixed with other dosage form products for use before flying prevention, the barrel mixing compatibility is good, and the abnormal problems of flocculation, layering and the like are not prone to occurring.

Description

Technical Field

[0001] The invention relates to the technical field of aqueous emulsions, and in particular to an aqueous emulsion containing benzylpyridamole and a preparation method thereof. Background Art

[0002] The country has put forward higher requirements for the green and environmental protection of agricultural production. The current development of water-based green and environmentally friendly pesticide formulations is also one of the environmental protection technologies advocated and strongly supported by the country. With the development of pesticide aerial spraying technology, pesticide herbicides are also required to have outstanding tank mixing effects and no tank mixing compatibility problems; and pesticide herbicides are required to have the characteristics of low toxicity, high efficiency, fast effect, low residue, and a wide range of applications, especially when mixed with other herbicides. The synergistic effect is obvious; benzylpyridinium has the characteristics of low toxicity, high efficiency, fast effect, low residue, and a wide range of applications, but benzylpyridinium is insoluble in water, and the molecular structure of benzylpyridinium contains ester bonds, which easily cause the risk of ester bond breakage in the molecule in the water system, causing benzylpyridinium to decompose, and it will make it difficult to ensure the stability of the water emulsion after it is made.

[0003] A Chinese patent with patent application number CN202210457620.2 discloses a dispersible oil suspension containing benzaclostrobin and a preparation method thereof. The patent solves the decomposition problem of benzaclostrobin in the dispersible oil suspension, but does not provide a solution to the problem of the stability of benzaclostrobin in the water system.

[0004] Therefore, providing an aqueous emulsion with good stability and capable of reducing the decomposition rate of benzylpyridamole is the main technical problem that needs to be solved at present. Summary of the invention

[0005] In order to solve the above technical problems, the first aspect of the present invention provides an aqueous emulsion containing benzylpyridinium, wherein the raw materials for its preparation include 5% to 30% of benzylpyridinium, 10% to 40% of solvent, 3% to 5% of emulsifier, 3% to 5% of antifreeze agent, 0.01% to 0.1% of defoamer, 0.1% to 1% of stabilizer, and the balance is water, in terms of mass percentage.

[0006] In one embodiment, the raw materials for its preparation include 10% to 20% of benzylpyridamole by mass percentage.

[0007] In one embodiment, the solvent includes a co-solvent and a main solvent, and the preparation raw material contains 10% to 15% of the co-solvent and 20% to 30% of the main solvent.

[0008] In one embodiment, the co-solvent is selected from one or a combination of capric amide and octanamide.

[0009] In one embodiment, the main solvent includes mineral spirits.

[0010] In one embodiment, the solvent oil is 150# solvent oil.

[0011] In one embodiment, the emulsifier includes one or a combination of EOPO block polyether and castor oil polyoxyethylene ether.

[0012] In one embodiment, the model of the EOPO block polyether includes but is not limited to one or more combinations of 5000HM, ETHYLAN NS-500LQ, and 1125.

[0013] In one embodiment, the types of castor oil polyoxyethylene ether include but are not limited to one or more combinations of EMULPON CO-360 and 3600B.

[0014] In one embodiment, the emulsifier includes a combination of castor oil polyoxyethylene ether with a model number of 3600B and EOPO block polyether with a model number of 1125.

[0015] In one embodiment, the emulsifier includes a combination of castor oil polyoxyethylene ether with a model number of EMULPON CO-360 and EOPO block polyether with a model number of ETHYLAN NS-500LQ.

[0016] In one embodiment, the emulsifier includes a combination of castor oil polyoxyethylene ether with model number EMULPON CO-360 and EOPO block polyether with model number 5000HM.

[0017] In one embodiment, the mass ratio of the castor oil polyoxyethylene ether to the EOPO block polyether is (1-3): (1-3).

[0018] In an optional embodiment, the mass ratio of the castor oil polyoxyethylene ether to the EOPO block polyether is 1.75:2.25.

[0019] In an optional embodiment, the mass ratio of the castor oil polyoxyethylene ether to the EOPO block polyether is 1:3.

[0020] In an optional embodiment, the mass ratio of the castor oil polyoxyethylene ether to the EOPO block polyether is 1.25:2.75.

[0021] In an optional embodiment, the mass ratio of the castor oil polyoxyethylene ether to the EOPO block polyether is 1:1.

[0022] In an optional embodiment, the mass ratio of the castor oil polyoxyethylene ether to the EOPO block polyether is 2.5:1.5.

[0023] In order to improve the storage stability of the aqueous emulsion containing benzylpyridinium, the inventors found during the experiment that when castor oil polyoxyethylene ether and EOPO block polyether are used for coordination, especially when the mass ratio of castor oil polyoxyethylene ether and EOPO block polyether is (1-3): (1-3), the stability of the aqueous emulsion containing benzylpyridinium can be improved, ensuring that the aqueous emulsion containing benzylpyridinium still has good stability after low-temperature storage and high-temperature storage.

[0024] In one embodiment, the stabilizer includes a combination of one or more of disodium hydrogen phosphate, triethanolamine, pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, and tris(2,4-di-tert-butylphenyl) phosphite.

[0025] In order to improve the stability of the aqueous emulsion containing benzylpyridinium, ensure that the aqueous emulsion containing benzylpyridinium has a shelf life stability of 2 years, and solve the problem that the ester bond will break when benzylpyridinium is developed into an aqueous emulsion, causing the decomposition rate of benzylpyridinium to be greater than 5%, the inventors found in the experiment that the stability of the aqueous emulsion containing benzylpyridinium can be improved after adding a stabilizer, but the inventors found that not all stabilizers can improve the stability of the aqueous emulsion containing benzylpyridinium and control the decomposition rate of benzylpyridinium to be less than 5%; when a specific castor oil polyoxyethylene ether and EOPO block polyether are used for compounding and then mixed with the stabilizer hydrogen phosphate The aqueous emulsion of benzathine obtained by compounding one or more combinations of disodium iodide, triethanolamine, pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, and tris(2,4-di-tert-butylphenyl) phosphite has good stability and can control the cleavage of the ester bond of benzathine in water, thereby leading to a high decomposition rate; the possible reason is that after adding a specific stabilizer and a specific emulsifier and controlling the pH value range of the aqueous emulsion containing benzathine, the decomposition rate of benzathine can be reduced to within 5%, the application effect of the aqueous emulsion containing benzathine is improved, and a qualified aqueous emulsion product is obtained.

[0026] In one embodiment, the stabilizer is disodium hydrogen phosphate, and the pH of the benzathine-containing aqueous emulsion is 7.2-7.80.

[0027] In a preferred embodiment, the stabilizer is disodium hydrogen phosphate, and the pH of the benzathine-containing aqueous emulsion is 7.51-7.70.

[0028] In order to make the aqueous emulsion containing benzylpyridinium have good storage stability and reduce the decomposition rate of benzylpyridinium in the aqueous emulsion containing benzylpyridinium during storage and at high temperature, so that the decomposition rate of benzylpyridinium is within 5%, the inventors accidentally found in the experiment that the pH value of the aqueous emulsion containing benzylpyridinium will change after adding a stabilizer. When the stabilizer is disodium hydrogen phosphate, it is combined with castor oil polyoxyethylene ether and EOPO block polyether to control the pH of the aqueous emulsion containing benzylpyridinium to 7.2-7.80, which will not affect the post-shear phase transition of the aqueous emulsion containing benzylpyridinium, and can reduce the decomposition rate of benzylpyridinium in the aqueous emulsion containing benzylpyridinium during storage and at high temperature; and when the pH of the aqueous emulsion containing benzylpyridinium is 7.51-7.70, the aqueous emulsion containing benzylpyridinium will not have the problem of demulsification and phase transition after storage at high temperature, and the decomposition rate of benzylpyridinium in the aqueous emulsion containing benzylpyridinium is controlled within 5%, so as to obtain qualified products.

[0029] In one embodiment, the stabilizer is triethanolamine, and the pH of the aqueous emulsion containing benzathine is 8.0-10.0.

[0030] In a preferred embodiment, the stabilizer is triethanolamine, and the pH of the benzathine-containing aqueous emulsion is 8.49-9.75.

[0031] The inventors unexpectedly discovered during the experiment that when triethanolamine is used as a stabilizer in combination with castor oil polyoxyethylene ether and EOPO block polyether, and the pH of the benzathine-containing aqueous emulsion is controlled to be 8.0-10.0, the benzathine-containing aqueous emulsion will not be affected by shear phase transition, and the decomposition rate of the benzathine-containing aqueous emulsion during storage and at high temperatures can be reduced, so that the decomposition rate of the benzathine-containing aqueous emulsion is controlled within 5%, and a qualified product is obtained. Moreover, the benzathine-containing aqueous emulsion will not have the problem of demulsification and phase transition after being stored at high temperatures, and a qualified product is obtained.

[0032] The stabilizer is one or a combination of tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]pentaerythritol and tris(2,4-di-tert-butylphenyl)phosphite, and the pH of the benzathine-containing aqueous emulsion is 5.0-6.0.

[0033] In one embodiment, the stabilizer is pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, and the pH of the aqueous emulsion containing benzathine is 5.0-6.0.

[0034] In one embodiment, the stabilizer is tris(2,4-di-tert-butylphenyl) phosphite, and the pH of the benzathine-containing aqueous emulsion is 5.0-6.0.

[0035] The inventors found in the experimental process that when pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate] or tris(2,4-di-tert-butylbenzene) phosphite is used as a stabilizer and is respectively matched with castor oil polyoxyethylene ether and EOPO block polyether, the pH of the aqueous emulsion containing benzathine is controlled to be 5.0-6.0, and the post-shear phase transition of the aqueous emulsion containing benzathine will not be affected, and the decomposition rate of the aqueous emulsion containing benzathine during storage and at high temperature can be reduced, so that the decomposition rate of benzathine in the aqueous emulsion containing benzathine is controlled within 5%, and a qualified product is obtained. Moreover, the aqueous emulsion containing benzathine will not have the problem of demulsification and phase transition after storage at high temperature.

[0036] The second aspect of the present invention provides a method for preparing a benzylpyridamole aqueous emulsion, comprising the following steps:

[0037] S1. The solvent is put into the oil phase autoclave, and then the benzylpyridazine and the emulsifier are sequentially added and stirred to obtain the oil phase;

[0038] S2. mixing water, antifreeze agent and defoamer to obtain an aqueous phase;

[0039] S3. adding the oil phase into the water phase for shearing, and adding a stabilizer for mixing to obtain a benzylpyridamole-containing aqueous emulsion.

[0040] In one embodiment, the particle size D of the aqueous emulsion containing benzylpyridamole obtained in S3 is 97 2~3μm.

[0041] In one embodiment, in S1, the solvent is added into the oil phase kettle, and then benzylpyridamole is added in sequence and heated to 50° C. to dissolve and clarify, and then an emulsifier is added and stirred to obtain an oil phase;

[0042] Beneficial Effects

[0043] 1. In the present application, disodium hydrogen phosphate is used as a stabilizer. When the pH of the aqueous emulsion containing benzathine is controlled to be 7.2-7.80, the aqueous emulsion containing benzathine will not be affected by the post-shear phase transition, and the decomposition rate of the aqueous emulsion containing benzathine during storage and at high temperatures can be reduced; and when the pH of the aqueous emulsion containing benzathine is 7.51-7.70, the aqueous emulsion containing benzathine will not have unstable problems such as water separation and stratification, demulsification and phase transition after storage at high temperatures, and a qualified product can be obtained.

[0044] 2. In the present application, triethanolamine is used as a stabilizer to cooperate with castor oil polyoxyethylene ether and EOPO block polyether. When the pH of the aqueous emulsion containing benzathine is controlled to 8.0-10.0, the aqueous emulsion containing benzathine will not have problems such as water separation and stratification, demulsification and phase transition during storage, and the decomposition rate of benzathine in the aqueous emulsion containing benzathine during storage and in a high-temperature storage environment can be reduced to less than 5%, thereby obtaining a qualified product.

[0045] 3. In the present application, when pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate] or tris(2,4-di-tert-butylbenzene) phosphite is used as a stabilizer and is respectively combined with castor oil polyoxyethylene ether and EOPO block polyether, the pH of the aqueous emulsion containing benzathine is controlled to be 5.0-6.0, which will not affect the post-shear phase transition of the aqueous emulsion containing benzathine, and the decomposition rate of benzathine in the aqueous emulsion containing benzathine during storage and at high temperature can be reduced to less than 5%, thereby obtaining a qualified product.

[0046] 4. In the present application, castor oil polyoxyethylene ether and EOPO block polyether are used for compounding, and the mass ratio of castor oil polyoxyethylene ether and EOPO block polyether is (1-3): (1-3). When the castor oil polyoxyethylene ether and EOPO block polyether are compounded with a stabilizer, the obtained aqueous emulsion containing benzylpyridinium chloride will not have problems of water separation, stratification, demulsification and phase transition during storage, which can improve the storage stability of the aqueous emulsion containing benzylpyridinium chloride and ensure that the aqueous emulsion containing benzylpyridinium chloride has a shelf life stability of 2 years.

[0047] 5. When the aqueous emulsion containing benzylpyridamole provided in the present application is diluted with water of different hardness and temperature, no flocculation, no stratification and no precipitation occur, which are all qualified. The aqueous emulsion containing benzylpyridamole has strong versatility and can be used for dilution and application with water in different regions.

[0048] 6. The aqueous emulsion containing benzylpyridamole provided in the present application has the characteristic of rapid weed control effect.

[0049] 7. The aqueous emulsion containing benzylpyridinium provided in the present application has good high-temperature storage stability, ensuring that the aqueous emulsion containing benzylpyridinium has a 2-year shelf life stability, and solves the problem that the ester bond will break when benzylpyridinium is developed into an aqueous emulsion, resulting in a decomposition rate of benzylpyridinium greater than 5%. BRIEF DESCRIPTION OF THE DRAWINGS

[0050] Figure 1 This is a diagram showing that the aqueous emulsion containing benzylpyridamole provided in the examples is in a normal state during storage.

[0051] Figure 2 This is a state diagram of the three samples of the aqueous emulsion containing benzylpyridamole provided in Example 3 showing water separation and stratification.

[0052] Figure 3This is a state diagram of the demulsification and phase transition of the benzathine-containing aqueous emulsion provided in Example 4.

[0053] Figure 4 This is a diagram showing the control effect of applying the benzathine emulsion provided in Example 7 to reeds.

[0054] Figure 5 These are pictures showing the control effect of the benzaclostrobin emulsion provided in Example 7 on goosegrass before and 3-7 days after application.

[0055] Figure 6 This is a graph showing the control effect of the benzaclostrobin emulsion provided in Example 7 on goosegrass 14-21 days after application.

[0056] Figure 7 These are pictures showing the control effect of the benzaclostrobin aqueous emulsion provided in Example 7 on Erigeron sphaerocephalus before and 3-7 days after application.

[0057] Figure 8 This is a graph showing the control effect of the benzaclostrobin aqueous emulsion provided in Example 7 on Erigeron australis 14-21 days after application. DETAILED DESCRIPTION

[0058] The sources of the raw materials used in the following examples are shown in Table 1.

[0059] Table 1

[0060]

[0061]

[0062] The first set of embodiments

[0063] The first group of embodiments provides a benzylpyridamole-containing aqueous emulsion, including embodiments 1-5, wherein the raw materials for its preparation include benzylpyridamole, solvent, emulsifier, antifreeze agent, defoaming agent, stabilizer, and water in percentage by mass; the difference between the raw materials for preparation in embodiments 1-5 is that the amount of stabilizer added is different, and the amount of water added is different, and the specific amounts added are shown in Table 1-1.

[0064] Table 1-1

[0065]

[0066] The stabilizer is disodium hydrogen phosphate.

[0067] The solvent is a combination of 10 wt % of an auxiliary solvent and 30 wt % of a main solvent.

[0068] The cosolvent is capric amide.

[0069] The main solvent is 150# solvent oil.

[0070] The emulsifier is a combination of castor oil polyoxyethylene ether with model number 3600B and EOPO block polyether with model number 1125; the mass ratio of castor oil polyoxyethylene ether with model number 3600B and EOPO block polyether with model number 1125 is 2.5:1.5.

[0071] The antifreeze agent is propylene glycol.

[0072] The model of the defoamer is Maitu SAG1572.

[0073] The water is deionized water.

[0074] The first group of embodiments provides a method for preparing a benzylpyridamole aqueous emulsion, comprising the following steps:

[0075] S1. The solvent is put into the oil phase autoclave, and then benzylpyridamole is added in sequence and heated to 50°C to dissolve and clarify, and then an emulsifier is added and stirred to obtain an oil phase;

[0076] S2. mixing water, antifreeze agent and defoamer to obtain an aqueous phase;

[0077] S3. Add the oil phase into the water phase for shearing, and add a stabilizer to mix evenly to obtain a benzylpyridamole-containing aqueous emulsion.

[0078] The particle size D of the aqueous emulsion containing benzylpyridamole obtained in Examples 1, 2, 3, 4 and 5 97 2~3μm.

[0079] Second set of embodiments

[0080] The second group of embodiments provides an aqueous emulsion containing benzylpyridamole, including embodiments 6-10, and its preparation raw materials include benzylpyridamole, solvent, emulsifier, antifreeze agent, defoaming agent, stabilizer, and water in percentage by mass; the difference in the preparation raw materials in embodiments 6-10 is that the added amount of stabilizer is different, the added amount of water is different, and the specific added amounts are shown in Table 2-1.

[0081] Table 2-1

[0082]

[0083] The stabilizer is triethanolamine.

[0084] The solvent includes 10 wt % of an auxiliary solvent and 30 wt % of a main solvent.

[0085] The cosolvent is capric amide.

[0086] The main solvent is 150# solvent oil.

[0087] The emulsifier is a combination of castor oil polyoxyethylene ether with model number EMULPON CO-360 and EOPO block polyether with model number ETHYLAN NS-500LQ; the mass ratio of castor oil polyoxyethylene ether with model number EMULPON CO-360 and EOPO block polyether with model number ETHYLAN NS-500LQ is 2.5:1.5.

[0088] The antifreeze agent is propylene glycol.

[0089] The model of the defoamer is Maitu SAG1572.

[0090] The water is deionized water.

[0091] The second group of embodiments provides a method for preparing a benzylpyridamole aqueous emulsion, comprising the following steps:

[0092] S1. The solvent is put into the oil phase autoclave, and then benzylpyridamole is added in sequence and heated to 50°C to dissolve and clarify, and then an emulsifier is added and stirred to obtain an oil phase;

[0093] S2. mixing water, antifreeze agent and defoamer to obtain an aqueous phase;

[0094] S3. Add the oil phase into the water phase for shearing, and add a stabilizer to mix evenly to obtain a benzylpyridamole-containing aqueous emulsion.

[0095] The particle size D of the aqueous emulsion containing benzylpyridamole obtained in Examples 6, 7, 8, 9 and 10 97 2~3μm.

[0096] The third group of embodiments

[0097] The third group of embodiments provides a benzylpyridamole-containing aqueous emulsion, including Embodiments 11-12. The raw materials for its preparation include benzylpyridamole, solvent, emulsifier, antifreeze agent, defoaming agent, stabilizer, and water in percentage by mass. The difference is that the type of stabilizer is different, and the specific addition amount is shown in Table 3-1.

[0098] Table 3-1

[0099]

[0100] The solvent includes 10 wt % of an auxiliary solvent and 30 wt % of a main solvent.

[0101] The cosolvent is capric amide.

[0102] The main solvent is 150# solvent oil.

[0103] The emulsifier is a combination of castor oil polyoxyethylene ether with model number EMULPON CO-360 and EOPO block polyether with model number 5000HM; the mass ratio of castor oil polyoxyethylene ether with model number EMULPON CO-360 and EOPO block polyether with model number 5000HM is 2.5:1.5.

[0104] The antifreeze agent is propylene glycol.

[0105] The model of the defoamer is Maitu SAG1572.

[0106] The water is deionized water.

[0107] The third group of embodiments provides a method for preparing a benzylpyridamole aqueous emulsion, comprising the following steps:

[0108] S1. The solvent is put into the oil phase autoclave, and then benzylpyridamole is added in sequence and heated to 50°C to dissolve and clarify, and then an emulsifier is added and stirred to obtain an oil phase;

[0109] S2. mixing water, antifreeze agent and defoamer to obtain an aqueous phase;

[0110] S3. Add the oil phase into the water phase for shearing, and add a stabilizer to mix evenly to obtain a benzylpyridamole-containing aqueous emulsion.

[0111] The particle size D of the aqueous emulsion containing benzylpyridamole obtained in Examples 11 and 12 97 2~3μm.

[0112] Fourth Group of Embodiments

[0113] The fourth group of embodiments provides a benzylpyridamole-containing aqueous emulsion, including embodiments 13-16. The raw materials for its preparation include benzylpyridamole, capric amide, 150# solvent oil, castor oil polyoxyethylene ether with model number 3600B, EOPO block polyether with model number 1125, antifreeze agent propylene glycol, defoamer Maitu SAG1572, stabilizer disodium hydrogen phosphate, and deionized water, and the specific addition amounts are shown in Table 4-1.

[0114] Table 4-1

[0115]

[0116] The fourth group of embodiments provides a method for preparing a benzylpyridamole-containing aqueous emulsion, and the specific implementation method is the same as the first group of embodiments.

[0117] The particle size D of the aqueous emulsion containing benzylpyridamole obtained in Examples 13, 14, 15 and 16 97 2~3μm.

[0118] Fifth Group of Embodiments

[0119] The fifth group of embodiments provides an aqueous emulsion containing benzylpyridinium, including embodiments 17-20. The raw materials for its preparation include benzylpyridinium, capric amide, 150# solvent oil, castor oil polyoxyethylene ether with model number EMULPON CO-360, EOPO block polyether with model number ETHYLAN NS-500LQ, antifreeze agent propylene glycol, defoamer Maitu SAG1572, stabilizer triethanolamine, and deionized water, and the specific addition amounts are shown in Table 5-1.

[0120] Table 5-1

[0121]

[0122] The fifth group of embodiments provides a method for preparing a benzylpyridamole-containing aqueous emulsion, and the specific implementation method is the same as the second group of embodiments.

[0123] The particle size D of the aqueous emulsion containing benzylpyridamole obtained in Examples 17, 18, 19 and 20 is 97 2~3μm.

[0124] Performance Testing

[0125] In the following performance tests, the benzathine emulsions in water provided in Examples 1-20 were stored in hot storage and cold storage. The hot storage condition was: 54°C±2°C for 14 days; the cold storage condition was: 0°C±2°C for 7 days.

[0126] The aqueous emulsion containing benzylpyridamole provided in the present disclosure needs to have a shelf life stability of 2 years. Using a time-temperature equivalence test scheme, placing it at 54° C. for 14 days is equivalent to the storage condition of a 2-year shelf life.

[0127] When the decomposition rate of the benzathine content in the benzathine emulsion after hot storage is less than 5%, it is a qualified product and can maintain shelf stability for 2 years.

[0128] 1. Storage stability test:

[0129] Observe whether the aqueous emulsion containing benzylpyridamole provided in the above Examples 1-20 will have water separation, stratification, demulsification and phase transition after hot storage and cold storage. If water separation, stratification and demulsification and phase transition occur, it is judged to be abnormal, and if water separation, stratification and demulsification and phase transition do not occur, it is judged to be normal. The test results of Examples 1-5 are shown in Table 1-2; the test results of Examples 6-10 are shown in Table 2-2; the test results of Examples 11 and 12 are shown in Table 3-2; the test results of Examples 13-16 are shown in Table 4-2; the test results of Examples 17-20 are shown in Table 5-2.

[0130] The normal state of the aqueous emulsion containing benzylpyridamole is shown in Figure 1 .

[0131] The state of water separation and stratification of the aqueous emulsion containing benzylpyridamole is shown in Figure 2 .

[0132] The state of demulsification and phase transition of the aqueous emulsion containing benzylpyridamole is shown in Figure 3 .

[0133] 2. pH test:

[0134] The pH of the benzathine-containing aqueous emulsions provided in Examples 1-12 at room temperature (25° C.) before storage was tested. The test results of Examples 1-5 are shown in Table 1-2; the test results of Examples 6-10 are shown in Table 2-2; and the test results of Examples 11 and 12 are shown in Table 3-2.

[0135] 3. Test of decomposition rate of benzothiazolin:

[0136] The decomposition rate of benzaclostrobin containing aqueous emulsions provided in Examples 1-12 was tested after 14 days of heat storage; the test results of Examples 1-5 are shown in Table 1-2; the test results of Examples 6-10 are shown in Table 2-2; the test results of Examples 11 and 12 are shown in Table 3-2.

[0137] The decomposition rate of fenpyroxil (%) = (1-the content of fenpyroxil after hot storage / the content of fenpyroxil in normal storage) * 100%.

[0138] 4. Applicability test:

[0139] The aqueous emulsions containing benzathine provided in Examples 2, 6, 7, 8, 9, 10, 11 and 12 were diluted with water of different temperatures and hardnesses, and their dilution stability was observed. When the observation results showed no flocculation, no stratification and no precipitation, they were determined to be qualified; when flocculation, stratification and precipitation occurred, they were determined to be unqualified. The test results are shown in 5-3.

[0140] 5. Weed control effect test:

[0141] The benzylpyridamole emulsion provided in Example 7 was applied to Phragmites australis, Goosegrass and Erigeron sphagnum to observe the effect of the application.

[0142] (1) Target of pesticide application: reed.

[0143] Application location: Nanpi County, Cangzhou City.

[0144] Application rate: 60mL / mu.

[0145] The weed control effect on reeds was tested before, 3 days after and 7 days after the application of pesticides. The test results are shown in Figure 4 .

[0146] (2) Target of pesticide application: Gnaphalium wilfordii.

[0147] Application location: Gaoqiao Town, Changsha County, Changsha City, Hunan Province.

[0148] Application rate: 60mL / mu.

[0149] The weed control effect on Goosegrass was tested before, 3 days after, 7 days after, 14 days after and 21 days after the application of pesticides. The test results are shown in Figure 5 and Figure 6 .

[0150] (3) Target of pesticide application: Erigeron cantoniensis.

[0151] Application location: Huanghua Town, Changsha County, Changsha City, Hunan Province.

[0152] Application rate: 60mL / mu.

[0153] The weed control effect on Erigeron edulis was tested before, 3 days, 7 days, 14 days and 21 days after the application of pesticides. The test results are shown in Figure 7 and Figure 8 .

[0154] pass Figure 4 It can be seen that the aqueous emulsion containing benzylpyridamole provided in the present application has the characteristic of rapid weed control on reeds.

[0155] pass Figure 5 and Figure 6 It can be seen that the aqueous emulsion containing benzylpyridamole provided in the present application has the characteristic of rapid weed control against sedge grass.

[0156] pass Figure 7 and Figure 8 It can be seen that the aqueous emulsion containing benzylpyraclostrobin provided in the present application has the characteristic of rapid weed control on Erigeron sphaerocephala.

[0157] Table 1-2

[0158]

[0159] It can be seen from Table 1-2 that the aqueous emulsion containing benzylpyridinium chloride obtained by using disodium hydrogen phosphate as a stabilizer in combination with benzylpyridinium chloride, when the amount of disodium hydrogen phosphate added is 0, the decomposition rate of benzylpyridinium chloride after hot storage is greater than 5%, which is an unqualified product. When the amount of disodium hydrogen phosphate added is 0.1%, it can play a stabilizing role, the hot storage decomposition rate is less than 5%, and the appearance is stable and normal; with the increase of the amount of disodium hydrogen phosphate, the decomposition rate of benzylpyridinium chloride after hot storage does not show a positively correlated decreasing trend; when the amount of disodium hydrogen phosphate added is greater than or equal to 0.3%, the aqueous emulsion containing benzylpyridinium chloride after hot storage suffers from unstable phenomena such as water separation and stratification, demulsification and phase transition; and the amount of disodium hydrogen phosphate added is greater than or equal to 0.3%. The addition amount will affect the pH of the benzathine emulsion in water. When the pH of the benzathine emulsion in water is controlled to be 7.2-7.80, it will not affect the water separation, stratification, demulsification and phase transition of the benzathine emulsion in water under cold storage, and the decomposition rate of the benzathine emulsion in water during storage and at high temperature can be reduced; and when the pH of the benzathine emulsion in water is 7.51-7.70, the benzathine emulsion in water will not have unstable problems such as water separation, stratification, demulsification and phase transition after storage at high temperature, and a qualified product can be obtained; when the addition amount of disodium hydrogen phosphate is 1wt%, the problem of demulsification and phase transition after shearing will occur in the process of preparing the benzathine emulsion in water.

[0160] Table 2-2

[0161]

[0162] It can be seen from Table 2-2 that when triethanolamine is used as a stabilizer in combination with EOPO block polyether and castor oil polyoxyethylene ether to control the pH of the benzathine emulsion to 8.0-10.0, the benzathine emulsion will not have problems such as water separation and stratification, demulsification and phase transition during storage, and the decomposition rate of the benzathine emulsion during storage and in a high-temperature storage environment can be reduced to less than 5%, thereby obtaining a qualified product. Furthermore, the benzathine emulsion will not have problems such as demulsification and phase transition after being stored at high temperature, thereby obtaining a qualified product.

[0163] Table 3-2

[0164]

[0165] It can be seen from Table 3-2 that when pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate] or tris(2,4-di-tert-butylbenzene) phosphite is used as a stabilizer and is respectively combined with EOPO block polyether and castor oil polyoxyethylene ether, and the pH of the benzathine emulsion in water is controlled to 5.0-6.0, the benzathine emulsion in water will not be affected by shear phase transition, and the benzathine decomposition rate of the benzathine emulsion in water under cold storage and hot storage can be reduced to less than 5%, and a qualified product can be obtained. Moreover, the benzathine emulsion in water will not have the problem of demulsification and phase transition after storage at high temperature, and a qualified product can be obtained. After 14 days of hot storage, the pH change is small, and benzathine is not decomposed, which improves the stability of the benzathine emulsion in water.

[0166] Table 4-2

[0167]

[0168] Table 5-2

[0169]

[0170] It can be seen from the test results in Table 4-2 and Table 5-2 that the aqueous emulsion containing benzylpyridinium chloride obtained by combining EOPO block polyether and castor oil polyoxyethylene ether in a mass ratio of (1 to 3): (1 to 3) with a stabilizer will not have problems such as water separation, stratification, demulsification and phase transition during cold storage and hot storage, which can improve the storage stability of the aqueous emulsion containing benzylpyridinium chloride and ensure that the aqueous emulsion containing benzylpyridinium chloride has a shelf life of 2 years.

[0171] Table 5-3

[0172]

[0173]

[0174] It can be seen from Table 5-3 that when the aqueous emulsions containing benzathine provided in Examples 2, 6, 7, 8, 9, 10, 11 and 12 of the present application are diluted with water of different hardness and temperature, no flocculation, no stratification and no precipitation occur, and all are in a qualified state. It can be seen that the aqueous emulsions containing benzathine provided in the above embodiments are highly versatile and can be used for dilution and application with water from different regions.

Claims

1. A water emulsion containing benzylpyridamole, characterized in that: Calculated by mass percentage, the preparation raw materials include 5% to 30% of benzylpyridamole, 10% to 40% of solvent, 3% to 5% of emulsifier, 3% to 5% of antifreeze agent, 0.01% to 0.1% of defoamer, 0.1% to 1% of stabilizer and the balance of water.

2. The aqueous emulsion containing benzylpyridamole according to claim 1, characterized in that: Calculated by mass percentage, the preparation raw materials include 10% to 20% of benzylpyridamole.

3. The aqueous emulsion containing benzylpyridamole according to claim 1, characterized in that: The emulsifier includes one or a combination of EOPO block polyether and castor oil polyoxyethylene ether.

4. The aqueous emulsion containing benzylpyridamole according to claim 3, characterized in that: The mass ratio of the castor oil polyoxyethylene ether to the EOPO block polyether is (1-3): (1-3).

5. The aqueous emulsion containing benzathine according to any one of claims 1 to 4, characterized in that: The stabilizer includes one or more combinations of disodium hydrogen phosphate, triethanolamine, pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, and tris(2,4-di-tert-butylphenyl) phosphite.

6. The aqueous emulsion containing benzylpyridamole according to claim 5, characterized in that: The stabilizer is disodium hydrogen phosphate, and the pH of the benzathine-containing aqueous emulsion is 7.2-7.

80.

7. The aqueous emulsion containing benzylpyridamole according to claim 5, characterized in that: The stabilizer is triethanolamine, and the pH of the benzathine-containing aqueous emulsion is 8.0-10.

0.

8. The aqueous emulsion containing benzylpyridamole according to claim 5, characterized in that: The stabilizer is one or a combination of tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]pentaerythritol and tris(2,4-di-tert-butylphenyl)phosphite, and the pH of the benzathine-containing aqueous emulsion is 5.0-6.

0.

9. A method for preparing the aqueous emulsion containing benzylpyridamole according to any one of claims 1 to 8, characterized in that: The following steps are involved: S1. The solvent is put into the oil phase autoclave, and then the benzylpyridazine and the emulsifier are sequentially added and stirred to obtain the oil phase; S2. mixing water, antifreeze agent and defoamer to obtain an aqueous phase; S3. adding the oil phase into the water phase for shearing, and adding a stabilizer for mixing to obtain a benzylpyridamole-containing aqueous emulsion.

10. The method for preparing the aqueous emulsion containing benzylpyridamole according to claim 9, characterized in that: The particle size D of the aqueous emulsion containing benzylpyridamole obtained in S3 97 2~3μm.

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