Preparation method of saflufenacil-containing microcapsule suspending agent as well as product and application of saflufenacil-containing microcapsule suspending agent
By controlling the temperature, pH value and dispersant type during the preparation of the phenylazole-containing microcapsule suspension agent, the problem of explosive accumulation is solved, the stability and fluidity of the product are achieved, and the application effect is ensured.
Patent Information
- Application Number
- CN202411690711.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-25
- Publication Date
- 2025-04-11
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of pesticide microcapsule suspensions, and in particular to a preparation method of a benzylpyridamole-containing microcapsule suspension, a product thereof and an application thereof. Background Art
[0002] With the adjustment of the country's pesticide policy, restrictions on the production and sales of highly toxic and high-residue pesticides, and the promotion of many environmental protection and resource conservation policies, the rise of high-efficiency agriculture and changes in farming systems have led to the development of pesticide formulations towards water-based, low-solvent, granular, slow-release and convenient directions. Microcapsule suspensions are sustained-release formulations with long lasting effects, stable active ingredients, reduced transdermal toxicity and environmental toxicity, reduced application times to reduce agricultural costs, and resource saving advantages. Microcapsule suspensions are safe, effective, and economical, and can be used as ideal pesticide formulations. The benefits they bring to economic development and social environment are immeasurable, and they have a very broad development prospect. They occupy an important position in pesticide formulations, and have specific advantages and broad development prospects. For microcapsule suspensions containing benzathine, benzathine is coated with concealed substances by adopting microcapsule coating technology, thereby isolating benzathine from the surrounding environment, thereby improving the stability of benzathine, extending the effective period of benzathine, and reducing transdermal toxicity and environmental toxicity. In addition, microcapsule suspensions containing benzathine are used for weed control in non-arable land and selective weeding in stem and leaf treatment, and will not cause pesticide damage to cultivated crops, and are highly safe. In particular, it can extend the duration of effect of benzaclostrobin, improve its stability, reduce transdermal toxicity and environmental toxicity, and reduce the number of times of application to reduce agricultural costs. In addition, the molecular structure of benzaclostrobin introduces uracil and isoxazoline groups at the same time, enriching the biological activity of benzaclostrobin, achieving a unique effect of controlling gramineous weeds with one drug, and has the characteristics of high efficiency in controlling broadleaf weeds, especially for grass weeds and sedge weeds, which can fill the gap in the control of glufosinate-ammonium and glyphosate-resistant weeds, and has a wide range of application scenarios and a wide range of weed control periods.
[0003] The Chinese patent with patent application number 201810259345.7 discloses a pesticide microcapsule suspension, its preparation method and application. The technical problems solved include that the capsule wall of the microcapsule suspension can protect the active ingredients of the pesticide from being decomposed by light, improve the efficacy and prolong the control time. However, it does not provide a solution to the problem of sudden aggregation that occurs during the preparation of the microcapsule suspension containing benzylpyridamole, which causes the sample to have poor fluidity or even become paste-like and not flowable, and the problem that it cannot be completely dispersed when diluted with water.
[0004] Therefore, the main technical problem that needs to be solved at present is to provide a method for preparing a microcapsule suspension containing benzylpyridazine, which can solve the problem of sudden aggregation during the preparation of the microcapsule suspension containing benzylpyridazine and the problem of poor fluidity of the sample or even the problem of paste-like stagnation. Summary of the invention
[0005] In the present application, benzylpyridinium is prepared into a microcapsule suspension, which can reduce the chemical decomposition of benzylpyridinium itself; the retention amount of benzylpyridinium microcapsules on the plant surface can be increased, the retention time can be prolonged, and the penetration ability to the plant epidermis can be improved, thereby achieving the purpose of improving the biological activity of benzylpyridinium, releasing the effective ingredients for a long time, reducing the number of times of application, liberating labor, and reducing the cost of pesticide use; however, the inventors found in the experimental process that abnormal problems may occur in the process of preparing the microcapsule suspension containing benzylpyridinium, and the problem of sudden aggregation is likely to occur during the preparation process or storage process, resulting in poor fluidity of the sample or even paste-like stagnant flow, and it cannot be completely dispersed after dilution with water, and a large amount of solid particles will sink to the bottom, which is easy to clog the nozzle during the application process, and the application of the drug cannot be normal, thereby affecting the efficacy of the product; it can be seen from this that solving the problem of sudden aggregation is particularly critical. The inventors conducted microscopic observations on the microcapsule suspension containing benzylpyridinium during the preparation process of the microcapsule suspension containing benzylpyridinium, thereby obtaining a microcapsule suspension containing benzylpyridinium with good stability and no adhesion, and good fluidity after hot storage, and no adhesion under the microscope.
[0006] The first aspect of the present invention provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0007] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0008] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0009] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added for modulation after heat preservation to obtain a microcapsule suspension containing benzylpyridamole;
[0010] The component B includes one or more combinations of emulsifier, dispersant, defoamer and water;
[0011] The component C comprises one or a combination of water-soluble capsule material and water;
[0012] The component D comprises a combination of one or more of a dispersant, a structure regulator, an antifreeze agent, and a preservative;
[0013] In S3, the temperature of adding component C dropwise into the emulsion for reaction is controlled to be ≤40°C.
[0014] In one embodiment, the temperature for adding component C dropwise into the emulsion for reaction in S3 is controlled to be 15-40°C.
[0015] In one embodiment, the temperature for insulation in S3 is 15-40° C., and the insulation time is 90 min.
[0016] In order to form the integrity and stability of the microcapsule suspension containing benzylpyridinium, and to avoid the reaction of isocyanate with water during the process of adding component C to the emulsion for reaction and solidification into capsules, the inventors found in the experimental process that it is necessary to control the pH value of the system when component C is added to the emulsion. The inventors creatively found in the experimental process that when the temperature of adding component C to the emulsion for reaction is controlled to be ≤40°C, especially when the temperature of adding component C to the emulsion for reaction is controlled to be 15-40°C, and the insulation temperature is 15-40°C, the pH value of the microcapsule suspension system in which component C is added to the emulsion for solidification into capsules can be effectively controlled. The possible reason is that when the temperature of adding component C to the emulsion for reaction exceeds 40°C, and the insulation temperature exceeds 40°C, the pH value of the microcapsule suspension system solidified into capsules will gradually increase, and the alkaline environment may catalyze the reaction of isocyanate and water, affecting the integrity and stability of the microcapsule suspension containing benzylpyridinium.
[0017] The solvent in the component A is 150# solvent oil.
[0018] The oil-soluble capsule material in the component A is isocyanate.
[0019] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0020] The emulsifier in the component B is a 20 wt % EOPO block polyether emulsifier aqueous solution.
[0021] The dispersant in the component B is a hydrophilic modified copolymer carboxylate dispersant.
[0022] The defoamer in the component B is defoamer SAG1572.
[0023] The water in the component B is deionized water.
[0024] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0025] The water-soluble capsule material in the component C is a polyamine; the polyamine is triethylenetetramine.
[0026] The water in the component C is deionized water.
[0027] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0028] The dispersant in the component D is a hydrophilic modified copolymer carboxylate dispersant.
[0029] The structural regulator in the component D is 2% liquid xanthan gum; the 2% liquid xanthan gum is obtained by dissolving xanthan gum in water, and the mass ratio of xanthan gum to water is 2:98.
[0030] The antifreeze agent in component D is ethylene glycol
[0031] The preservative in component D is sodium benzoate.
[0032] The specific raw material compositions and mass proportions of component A, component B, component C, and component D are shown in Table 1.
[0033] Table 1
[0034]
[0035]
[0036] In one embodiment, the purity of the benzathine is 92%.
[0037] In Table 1, the proportion of benzaclostrobin is ((10 / 0.92)%), which means that benzaclostrobin with a purity of 92% is added in an amount equivalent to 10% of the actual feed.
[0038] In one embodiment, the isocyanate is a combination of 80 wt% 2,4-TDI and 20 wt% 2,6-TDI.
[0039] The inventors found during the experiment that when a phosphate dispersant and a hydrophilic modified copolymer carboxylate dispersant are used in combination, the problem of violent aggregation will easily occur when component C is added dropwise into the emulsion for solidification into capsules. When a hydrophilic modified copolymer carboxylate dispersant is used to replace the dispersant obtained by compounding a phosphate dispersant and a hydrophilic modified copolymer carboxylate dispersant, the problem of violent aggregation that will easily occur during solidification into capsules can be solved.
[0040] The inventors found during the experiment that when an emulsifier is added to the oil phase (component A), the stability of the emulsion can be improved. When the emulsifier is added to the oil phase, the reaction liquid in the solidification capsule stage is more viscous. The emulsifier can also be made into a 20% aqueous solution for use.
[0041] The inventors found in the experimental process that when the mass ratio of oil-soluble capsule material to water-soluble capsule material is 6:1, the problem of component C being prone to violent polymerization when added dropwise to the emulsion for solidification into capsules can be improved.
[0042] The inventors found in the experimental process that when the temperature of the emulsion is higher than 40°C, the pH value of the emulsion exceeds 10, which affects the stability of the microcapsule suspension containing benzylpyridamole during solidification and encapsulation.
[0043] In one embodiment, the stirring speed of adding component A into component B for stirring and shearing in S2 is 290-465 r / min.
[0044] In one embodiment, the emulsion in S3 is added with component C at a stirring speed of 290-465 r / min, and the stirring speed during heat preservation in S3 is 290-465 r / min.
[0045] The technical resistance problem encountered by the inventors during the experiment is that when component C formed by water-soluble capsule material and water is added dropwise to the emulsion, it will affect the stability of the microcapsule suspension containing benzylpyrimidine azole solidified into capsules. The inventors found during the experiment that when the dropwise acceleration of component C added to the emulsion is too fast and the stirring speed is low, the emulsion and component C formed by water-soluble capsule material and water react with agglomeration and adhesion, and local paste appears, and dilution with water cannot be completely dispersed. And the inventors found during the experiment that when component C is added dropwise to the emulsion for stirring and shearing to solidify into capsules, the stirring and shearing speed of stirring and shearing needs to be maintained at 290-465r / min to improve the stability of the microcapsule suspension containing benzylpyrimidine azole solidified into capsules. The possible reason is that when the stirring and shearing speed of stirring and shearing needs to be maintained at 290-465r / min, component C can be added dropwise to the emulsion to present a vortex flow and a dead angle-free state, thereby improving the stability of the microcapsule suspension containing benzylpyrimidine azole solidified into capsules.
[0046] In one embodiment, the emulsion in S3 is dripped with component C at a stirring speed of 290-465 r / min, and the dripping stage of component C into the emulsion includes at least one dripping stage.
[0047] In one embodiment, the dripping time in the dripping stage in S3 is 30-90 min.
[0048] In one embodiment, the dripping time in the dripping stage in S3 includes but is not limited to 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min, 40min, 41min, 42min, 43min, 44min, 45min, 46min, 47min, 48min, 49min, 50min, 51min, 52min, 53min, 54min, 55min, 56min, 57min, 58min, 59min, 60min, 61min, 62min, 63min, 64min, 65min, 66min, 67min, 68min, 69min, 70min, 71min, 72min, 73min, 74m in, 75min, 76min, 77min, 78min, 79min, 80min, 81min, 82min, 83min, 84min, 85min, 86min, 87min, 88min, 89min, 90min.
[0049] In one embodiment, the time required to pause during the process of adding component C dropwise to the emulsion in S3 is 0-30 minutes.
[0050] In one embodiment, the time required to pause during the process of adding component C dropwise to the emulsion in S3 includes but is not limited to 0 min, 1 min, 2 min, 3 min, 4 min, 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, 16 min, 17 min, 18 min, 19 min, 20 min, 21 min, 22 min, 23 min, 24 min, 25 min, 26 min, 27 min, 28 min, 29 min, and 30 min.
[0051] The technical obstacles encountered by the inventors during the experiment are that in the process of preparing the microcapsule suspension containing benzylpyridinium, there will be problems of sudden aggregation after backlog or local paste problem, resulting in the failure to obtain qualified microcapsule suspension containing benzylpyridinium; during the experiment, the inventors found that the time of starting to drip component C formed by water-soluble capsule material and water in the emulsion should be strictly controlled, and the solidification capsule process should be started as soon as possible, otherwise it will cause the oil-soluble capsule material to hydrolyze, causing the risk of self-aggregation and sudden aggregation; and the inventors found during the experiment that when component C is dripped into the emulsion, the dripping time of component C needs to be controlled. When the dropping time of component C is short, the dropping speed of component C will be fast. During the dropping process, component C and the raw materials in the emulsion will not have time to react, and there will be a problem of sudden aggregation after accumulation or a problem of local creaming, leading to failure; when the dropping time of component C is long, it will cause hydrolysis of the oil-soluble capsule material, thereby causing the risk of self-aggregation and sudden aggregation, and there will also be a problem of local creaming; the inventors found that when the dropping time of the dropping stage in S3 is 30-90min, and the pause time during the dropping process of adding component C to the emulsion is 0-30min, the problems of local creaming and sudden aggregation can be avoided.
[0052] In one embodiment, the step of adding component C to the emulsion in S3 includes one dropping step, two dropping steps, three dropping steps, four dropping steps, or five dropping steps.
[0053] During the experiment, the inventors found that the dripping time and amount of component C added to the emulsion need to be controlled. If necessary, it is necessary to pause for a while before dripping component C, and control the dripping speed of component C into the emulsion to achieve a suitable dripping reaction state to avoid causing hydrolysis of the oil-soluble capsule material and inducing the risk of self-aggregation and violent aggregation.
[0054] In one embodiment, the dripping time of the single dripping stage is 30-90min, and the dripping amount of the single dripping is 100wt% of component C; the dripping time of the single dripping stage includes but is not limited to 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min, 40min, 41min, 42min, 43min, 44min, 45min, 46min, 47min, 48min, 49min, 50min, 51min, 52min, 53min, 54 min, 55min, 56min, 57min, 58min, 59min, 60min, 61min, 62min, 63min, 64min, 65min, 66min, 67min, 68min, 69min, 70min, 71min, 72mi n, 73min, 74min, 75min, 76min, 77min, 78min, 79min, 80min, 81min, 82min, 83min, 84min, 85min, 86min, 87min, 88min, 89min, 90min.
[0055] In one embodiment, the dropping sequence of the secondary dropping stage includes a first dropping stage, a first pause stage, and a second dropping stage; the dropping time of the first dropping stage is 20-25min, the dropping amount of the first dropping stage is 50-65wt% of component C, the pause time of the first pause stage is 4-10min, the dropping time of the second dropping stage is 10-15min, and the dropping amount of the second dropping stage is the remaining component C.
[0056] In one embodiment, the dropping time of the first dropping stage in the secondary dropping stage includes but is not limited to 20min, 21min, 22min, 23min, 24min, 25min; the pause time of the first pause stage in the secondary dropping stage includes but is not limited to 4min, 5min, 6min, 7min, 8min, 9min, 10min; the dropping time of the second dropping stage in the secondary dropping stage includes but is not limited to 10min, 11min, 12min, 13min, 14min, 15min.
[0057] In one embodiment, the dropping sequence of the three dropping stages includes a first dropping stage, a first pause stage, a second dropping stage, a second pause stage, and a third dropping stage; the dropping time of the first dropping stage is 25-35min, the dropping amount of the first dropping stage is 70-75wt% of component C, the pause time of the first pause stage is 3-8min, the dropping time of the second dropping stage is 5-10min, the dropping amount of the second dropping stage is 12-20wt% of component C, the pause time of the second pause stage is 3-8min, the dropping time of the third dropping stage is 3-8min, and the dropping amount of the third dropping stage is the remaining component C.
[0058] In one embodiment, the dropping time of the first dropping stage in the three dropping stages includes but is not limited to 25min, 26min, 27min, 28min, 29min, 30min, 31min, 32min, 33min, 34min, 35min; the pause time of the first pause stage in the three dropping stages includes but is not limited to 3min, 4min, 5min, 6min, 7min, 8min; the dropping time of the second dropping stage in the three dropping stages includes but is not limited to 5min, 6min, 7min, 8min, 9min, 10min; the pause time of the second pause stage in the three dropping stages includes but is not limited to 3min, 4min, 5min, 6min, 7min, 8min; the dropping time of the third dropping stage in the three dropping stages includes but is not limited to 3min, 4min, 5min, 6min, 7min, 8min.
[0059] In one embodiment, the dropping sequence of the four dropping stages includes a first dropping stage, a first pause stage, a second dropping stage, a second pause stage, a third dropping stage, a third pause stage, and a fourth dropping stage; the dropping time of the first dropping stage is 20-30 min, the dropping amount of the first dropping stage is 55-63 wt% of component C, the pause time of the first pause stage is 3-8 min, the dropping time of the second dropping stage is 5-10 min, the dropping amount of the second dropping stage is 15-24 wt% of component C, the pause time of the second pause stage is 3-8 min, the dropping time of the third dropping stage is 1-8 min, the dropping amount of the third dropping stage is 6-12 wt% of component C, the pause time of the third pause stage is 1-8 min, the dropping time of the fourth dropping stage is 1-8 min, and the dropping amount of the fourth dropping stage is the remainder component C.
[0060] In one embodiment, the dripping time of the first dripping stage in the four dripping stages includes but is not limited to 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min, 30min; the pause time of the first pause stage in the four dripping stages includes but is not limited to 3min, 4min, 5min, 6min, 7min, 8min; the dripping time of the second dripping stage in the four dripping stages includes but is not limited to 5min, 6min, 7min, 8min, 9min, 10min; the pause time of the second pause stage in the four dripping stages includes but is not limited to 15min, 20min, 21min, 22min, 23min, 24min, 25min, 26min, 27min, 28min, 29min, 30min. The dropping time of the third dropping stage in the four dropping stages includes but is not limited to 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min; the pause time of the three pause stages in the four dropping stages includes but is not limited to 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min; the dropping time of the fourth dropping stage in the four dropping stages includes but is not limited to 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min.
[0061] In one embodiment, the order of the five dropping stages includes a first dropping stage, a pause stage, a second dropping stage, a second pause stage, a third dropping stage, a third pause stage, a fourth dropping stage, a fourth pause stage, and a fifth dropping stage; the dropping time of the first dropping stage is 28-35min, the dropping amount of the first dropping stage is 75-80wt% of component C, the pause time of the first pause stage is 6-12min, the dropping time of the second dropping stage is 0.5-3min, and the dropping amount of the second dropping stage is 1-5wt% of component C, the pause time of the second pause stage is 3-8min, the dropping time of the third dropping stage is 0.5-3min, the dropping amount of the third dropping stage is 1-5wt% of component C, the pause time of the third pause stage is 1-5min, the dropping time of the fourth dropping stage is 0.5-4min, the dropping amount of the fourth dropping stage is 2-8wt% of component C, the pause time of the fourth pause stage is 1-8min, the dropping time of the fifth dropping stage is 1-8min, and the dropping amount of the fourth dropping stage is the remainder component C.
[0062] In one embodiment, the dripping time of the first dripping stage in the five dripping stages includes but is not limited to 28min, 29min, 30min, 31min, 32min, 33min, 34min, 35min; the pause time of the first pause stage in the five dripping stages includes but is not limited to 6min, 7min, 8min, 9min, 10min, 11min, 12min; the dripping time of the second dripping stage in the five dripping stages includes but is not limited to 0.5min, 1min, 1.5min, 2min, 2.5min, 3min; the pause time of the second pause stage in the five dripping stages includes but is not limited to 3min, 4min, 5min, 6min, 7min, 8min; the dripping time of the third dripping stage in the five dripping stages includes but is not limited to The pause time of the three pause stages in the five dropping stages includes but is not limited to 1min, 2min, 3min, 4min, 5min; the dropping time of the fourth dropping stage in the five dropping stages includes but is not limited to 0.5min, 1min, 1.5min, 2min, 2.5min, 3min, 3.5min, 4min; the pause time of the four pause stages in the five dropping stages includes but is not limited to 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min; the dropping time of the fifth dropping stage in the five dropping stages includes but is not limited to 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min.
[0063] The second aspect of the present invention provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0064] The inventor found in the experiment that when the oil-soluble isocyanate used in the capsule material is exposed to moisture in the air for a long time, it is easy to decompose and self-polymerize, causing the material to deteriorate and the barrel lid to be unable to open normally. Therefore, it is recommended to wipe the mouth of the packaging barrel clean after using the isocyanate and quickly close the barrel lid for storage.
[0065] The third aspect of the present invention provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0066] Beneficial Effects
[0067] In the present application, benzathine is prepared into a microcapsule suspension, which can reduce the chemical decomposition of benzathine itself; increase the retention amount of benzathine microcapsules on the plant surface, prolong the retention time and improve the penetration ability into the plant epidermis, thereby achieving the purpose of improving the biological activity of benzathine, releasing the active ingredients for a long time, reducing the number of applications, liberating labor and reducing the cost of pesticide use.
[0068] In the present application, when component C is added dropwise to the emulsion for stirring and shearing to solidify into capsules, the stirring and shearing speed needs to be maintained at 290-465r / min to improve the stability of the solidified capsules to form a microcapsule suspension containing benzathine. The possible reason is that when the stirring and shearing speed needs to be maintained at 290-465r / min, component C can be added dropwise to the emulsion to present a vortex flow without dead ends, thereby improving the stability of the solidified capsules to form a microcapsule suspension containing benzathine.
[0069] In the present application, when the dripping time of component C is long, it will cause hydrolysis of the oil-soluble capsule material, thereby causing the risk of self-aggregation and violent aggregation, and the problem of local creaming will also occur; the inventors found that when the dripping time of the dripping stage in S3 is 30-90 minutes, and the pause time during the dripping process of adding component C to the emulsion is 0-30 minutes, the problems of local creaming and violent aggregation can be avoided.
[0070] In the present application, the dripping time and the dripping amount of component C added to the emulsion need to be controlled. If necessary, it is necessary to pause for a while before dripping component C, and control the dripping speed of component C to the emulsion to achieve a suitable dripping reaction state to avoid causing hydrolysis of the oil-soluble capsule material and inducing the risk of self-aggregation and violent aggregation.
[0071] In the present application, when a phosphate dispersant and a hydrophilic modified copolymer carboxylate dispersant are used in combination, the problem of sudden aggregation will easily occur when component C is added dropwise into the emulsion for solidification into capsules. When a hydrophilic modified copolymer carboxylate dispersant is used to replace the dispersant obtained by compounding a phosphate dispersant and a hydrophilic modified copolymer carboxylate dispersant, the problem of sudden aggregation that will easily occur during solidification into capsules can be solved. BRIEF DESCRIPTION OF THE DRAWINGS
[0072] Figure 1 After hot storage, the microscopic observation showed that there was no agglomeration or adhesion.
[0073] Figure 2 After hot storage, microscopic observation revealed that problems of agglomeration and adhesion and violent aggregation had occurred.
[0074] Figure 3 Microscopic observation after cold storage revealed problems of agglomeration and adhesion, as well as violent aggregation.
[0075] Figure 4 It is a state in which the problem of sudden aggregation occurs during the preparation process.
[0076] Figure 5 This is the sample bottle used for hot storage.
[0077] Figure 6 This is a sample bottle used for cold storage. DETAILED DESCRIPTION
[0078] The raw material composition and addition amount involved in the following experimental groups are shown in Table 2.
[0079] Table 2
[0080]
[0081] The purity of the benzylpyridamole is 92%.
[0082] In Table 2, the proportion of benzaclostrobin is (10 / 0.92)%, which means that benzaclostrobin with a purity of 92% is added in an amount equivalent to 10% of the actual feed.
[0083] The 2% liquid xanthan gum in Table 2 is obtained by dissolving xanthan gum in water, and the mass ratio of xanthan gum to water is 2:98.
[0084] The solvent of the 20 wt % EOPO block polyether emulsifier aqueous solution is water, and the solute is the EOPO block polyether emulsifier.
[0085] The conditions for uniform mixing in the following experimental groups are all that the raw materials are mixed at 25°C.
[0086] The manufacturers and models of the raw materials involved in the following experimental groups are shown in Table 3.
[0087] Table 3
[0088]
[0089] The 2,4-TDI is 2,4-toluene diisocyanate, and the 2,6-TDI is 2,6-toluene diisocyanate.
[0090] The first set of experiments
[0091] The first set of experiments included Example 1 and Example 2.
[0092] Example 1
[0093] The first aspect of the present embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0094] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0095] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0096] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added for modulation after heat preservation to obtain a microcapsule suspension containing benzylpyridamole;
[0097] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0098] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0099] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0100] The specific names and amounts of raw materials used are shown in Table 2.
[0101] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 19.4°C.
[0102] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 293 r / min.
[0103] The emulsion in S3 is dripped with component C at a stirring speed of 293 r / min, and the dripping stage of component C into the emulsion is a single dripping stage; the dripping time of the single dripping stage is 30 min, and the dripping amount of the single dripping is 100 wt% of component C.
[0104] The temperature for heat preservation in S3 is 20° C., the stirring speed during heat preservation in S3 is 293 r / min, and the heat preservation time is 90 min.
[0105] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0106] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0107] Example 2
[0108] The first aspect of this embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of Example 1, except that:
[0109] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 21.4°C.
[0110] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 416 r / min.
[0111] The emulsion in S3 is dripped with component C at a stirring speed of 416 r / min, and the dripping stage of component C into the emulsion is a single dripping stage; the dripping time of the single dripping stage is 30 min, and the dripping amount of the single dripping is 100 wt% of component C.
[0112] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0113] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0114] The second set of experiments
[0115] The second group of experiments includes Example 3, Example 4, Example 5, and Example 6.
[0116] Example 3
[0117] The first aspect of the present embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0118] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0119] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0120] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0121] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0122] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0123] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0124] The specific names and amounts of raw materials used are shown in Table 2.
[0125] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 17.4°C.
[0126] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 348 r / min.
[0127] The emulsion in S3 is dripped with component C at a stirring speed of 348 r / min, and the dripping stage of component C being dripped into the emulsion is a secondary dripping stage; the dripping sequence of the secondary dripping stage includes a first dripping stage, a first pause stage, and a second dripping stage; the dripping time of the first dripping stage is 21 min, the dripping amount of the first dripping stage is 65 wt% of component C, the pause time of the first pause stage is 9 min, the dripping time of the second dripping stage is 11 min, and the dripping amount of the second dripping stage is the remaining component C.
[0128] The temperature for heat preservation in S3 is 17.4° C., the stirring speed during heat preservation in S3 is 348 r / min, and the heat preservation time is 90 min.
[0129] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0130] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0131] Example 4
[0132] The first aspect of this embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method thereof is the same as that of Example 3, except that:
[0133] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 19.5°C.
[0134] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 370 r / min.
[0135] The emulsion in S3 is dripped with component C at a stirring speed of 370r / min, and the dripping stage of component C being dripped into the emulsion is a secondary dripping stage; the dripping sequence of the secondary dripping stage includes a first dripping stage, a first pause stage, and a second dripping stage; the dripping time of the first dripping stage is 21min, the dripping amount of the first dripping stage is 65wt% of component C, the pause time of the first pause stage is 9min, the dripping time of the second dripping stage is 11min, and the dripping amount of the second dripping stage is the remaining component C.
[0136] The temperature for heat preservation in S3 is 19.5° C., the stirring speed during heat preservation in S3 is 370 r / min, and the heat preservation time is 90 min.
[0137] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0138] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0139] Example 5
[0140] The first aspect of the present embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0141] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0142] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0143] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0144] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0145] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0146] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0147] The specific names and amounts of raw materials used are shown in Table 2.
[0148] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 18.4°C.
[0149] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 371 r / min.
[0150] The emulsion in S3 is dripped with component C at a stirring speed of 371r / min, and the dripping stage of component C into the emulsion is a secondary dripping stage; the dripping sequence of the secondary dripping stage includes a first dripping stage, a first pause stage, and a second dripping stage; the dripping time of the first dripping stage is 21min, the dripping amount of the first dripping stage is 50wt% of component C, the pause time of the first pause stage is 5min, the dripping time of the second dripping stage is 10min, and the dripping amount of the second dripping stage is the remaining component C.
[0151] The temperature for heat preservation in S3 is 18.4° C., the stirring speed during heat preservation in S3 is 371 r / min, and the heat preservation time is 90 min.
[0152] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0153] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0154] Example 6
[0155] The first aspect of this embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of Example 5, except that:
[0156] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 19.1°C.
[0157] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 400 r / min.
[0158] The emulsion in S3 is dripped with component C at a stirring speed of 400r / min, and the dripping stage of component C being dripped into the emulsion is a secondary dripping stage; the dripping sequence of the secondary dripping stage includes a first dripping stage, a first pause stage, and a second dripping stage; the dripping time of the first dripping stage is 21min, the dripping amount of the first dripping stage is 50wt% of component C, the pause time of the first pause stage is 5min, the dripping time of the second dripping stage is 10min, and the dripping amount of the second dripping stage is the remaining component C.
[0159] The temperature for heat preservation in S3 is 19.1° C., the stirring speed during heat preservation in S3 is 400 r / min, and the heat preservation time is 90 min.
[0160] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0161] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0162] The third group of experiments
[0163] The third group of experiments includes Example 7 and Example 8.
[0164] Example 7
[0165] The first aspect of the present embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0166] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0167] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0168] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0169] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0170] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0171] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0172] The specific names and amounts of raw materials used are shown in Table 2.
[0173] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 22.5°C.
[0174] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 400 r / min.
[0175] The emulsion in S3 is dripped with component C at a stirring speed of 400r / min, and the dripping stages of component C being dripped into the emulsion are three dripping stages; the dripping sequence of the three dripping stages includes a first dripping stage, a first pause stage, a second dripping stage, a second pause stage, and a third dripping stage; the dripping time of the first dripping stage is 30min, the dripping amount of the first dripping stage is 71.43wt% of component C, the pause time of the first pause stage is 5min, the dripping time of the second dripping stage is 7min, the dripping amount of the second dripping stage is 16.67wt% of component C, the pause time of the second pause stage is 5min, the dripping time of the third dripping stage is 5min, and the dripping amount of the third dripping stage is the remainder component C.
[0176] The temperature for heat preservation in S3 is 22.5° C., the stirring speed during heat preservation in S3 is 400 r / min, and the heat preservation time is 90 min.
[0177] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0178] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0179] Example 8
[0180] The first aspect of this embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of Example 7, except that:
[0181] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 24.5°C.
[0182] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 460 r / min.
[0183] The emulsion in S3 is dripped with component C at a stirring speed of 460r / min, and the dripping stages of component C being dripped into the emulsion are three dripping stages; the dripping sequence of the three dripping stages includes a first dripping stage, a first pause stage, a second dripping stage, a second pause stage, and a third dripping stage; the dripping time of the first dripping stage is 30min, the dripping amount of the first dripping stage is 71.43wt% of component C, the pause time of the first pause stage is 5min, the dripping time of the second dripping stage is 7min, the dripping amount of the second dripping stage is 16.67wt% of component C, the pause time of the second pause stage is 5min, the dripping time of the third dripping stage is 5min, and the dripping amount of the third dripping stage is the remainder component C.
[0184] The temperature for heat preservation in S3 is 24.5° C., the stirring speed during heat preservation in S3 is 460 r / min, and the heat preservation time is 90 min.
[0185] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0186] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0187] The fourth experiment
[0188] The fourth group of experiments includes Example 9, Example 10, Example 11, and Example 12.
[0189] Example 9
[0190] The first aspect of the present embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0191] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0192] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0193] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0194] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0195] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0196] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0197] The specific names and amounts of raw materials used are shown in Table 2.
[0198] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 21.8°C.
[0199] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 455 r / min.
[0200] The emulsion in S3 is dripped with component C at a stirring speed of 455r / min, and the dripping stage of component C dripping into the emulsion is four dripping stages; the dripping order of the four dripping stages includes a first dripping stage, a first pause stage, a second dripping stage, a second pause stage, a third dripping stage, a third pause stage, and a fourth dripping stage; the dripping time of the first dripping stage is 27min, the dripping amount of the first dripping stage is 62.26wt% of component C, the pause time of the first pause stage is 5min, the dripping time of the second dripping stage is 5min, the dripping amount of the second dripping stage is 17.15wt% of component C, the pause time of the second pause stage is 5min, the dripping time of the third dripping stage is 2min, the dripping amount of the third dripping stage is 6.86wt% of component C, the pause time of the three pause stages is 2min, the dripping time of the fourth dripping stage is 4min, and the dripping amount of the fourth dripping stage is the remainder component C.
[0201] The temperature for heat preservation in S3 is 21.8° C., the stirring speed during heat preservation in S3 is 455 r / min, and the heat preservation time is 90 min.
[0202] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0203] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0204] Example 10
[0205] The first aspect of this embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of Example 9, except that:
[0206] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 23.9°C.
[0207] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 461 r / min.
[0208] The emulsion in S3 is dripped with component C at a stirring speed of 461r / min, and the dripping stage of component C dripping into the emulsion is four dripping stages; the dripping order of the four dripping stages includes a first dripping stage, a first pause stage, a second dripping stage, a second pause stage, a third dripping stage, a third pause stage, and a fourth dripping stage; the dripping time of the first dripping stage is 27min, the dripping amount of the first dripping stage is 62.26wt% of component C, the pause time of the first pause stage is 5min, the dripping time of the second dripping stage is 5min, the dripping amount of the second dripping stage is 17.15wt% of component C, the pause time of the second pause stage is 5min, the dripping time of the third dripping stage is 2min, the dripping amount of the third dripping stage is 6.86wt% of component C, the pause time of the three pause stages is 2min, the dripping time of the fourth dripping stage is 4min, and the dripping amount of the fourth dripping stage is the remainder component C.
[0209] The temperature for heat preservation in S3 is 23.9° C., the stirring speed during heat preservation in S3 is 461 r / min, and the heat preservation time is 90 min.
[0210] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0211] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0212] Embodiment 11
[0213] The first aspect of the present embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0214] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0215] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0216] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0217] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0218] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0219] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0220] The specific names and amounts of raw materials used are shown in Table 2.
[0221] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 25.4°C.
[0222] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 450 r / min.
[0223] The emulsion in S3 is dripped with component C at a stirring speed of 450r / min, and the dripping stage of component C dripping into the emulsion is four dripping stages; the dripping order of the four dripping stages includes a first dripping stage, a first pause stage, a second dripping stage, a second pause stage, a third dripping stage, a third pause stage, and a fourth dripping stage; the dripping time of the first dripping stage is 23min, the dripping amount of the first dripping stage is 55wt% of component C, the pause time of the first pause stage is 5min, the dripping time of the second dripping stage is 10min, the dripping amount of the second dripping stage is 23.8wt% of component C, the pause time of the second pause stage is 5min, the dripping time of the third dripping stage is 5min, the dripping amount of the third dripping stage is 11.7wt% of component C, the pause time of the three pause stages is 5min, the dripping time of the fourth dripping stage is 4min, and the dripping amount of the fourth dripping stage is the remainder component C.
[0224] The temperature for heat preservation in S3 is 25.4° C., the stirring speed during heat preservation in S3 is 450 r / min, and the heat preservation time is 90 min.
[0225] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0226] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0227] Example 12
[0228] The first aspect of this embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of Example 11, except that:
[0229] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 23.2°C.
[0230] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 456 r / min.
[0231] The emulsion in S3 is dripped with component C at a stirring speed of 456r / min, and the dripping stage of component C dripping into the emulsion is four dripping stages; the dripping order of the four dripping stages includes a first dripping stage, a first pause stage, a second dripping stage, a second pause stage, a third dripping stage, a third pause stage, and a fourth dripping stage; the dripping time of the first dripping stage is 23min, the dripping amount of the first dripping stage is 55wt% of component C, the pause time of the first pause stage is 5min, the dripping time of the second dripping stage is 10min, the dripping amount of the second dripping stage is 23.8wt% of component C, the pause time of the second pause stage is 5min, the dripping time of the third dripping stage is 5min, the dripping amount of the third dripping stage is 11.7wt% of component C, the pause time of the three pause stages is 5min, the dripping time of the fourth dripping stage is 4min, and the dripping amount of the fourth dripping stage is the remainder component C.
[0232] The temperature for heat preservation in S3 is 23.2° C., the stirring speed during heat preservation in S3 is 456 r / min, and the heat preservation time is 90 min.
[0233] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0234] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0235] The fifth experiment
[0236] The fifth group of experiments includes Example 13 and Example 14.
[0237] Embodiment 13
[0238] The first aspect of the present embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0239] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0240] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0241] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0242] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0243] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0244] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0245] The specific names and amounts of raw materials used are shown in Table 2.
[0246] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 17.4°C.
[0247] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 293 r / min.
[0248] The emulsion in S3 is dripped with component C at a stirring speed of 293 r / min, and the dripping stage of component C dripping into the emulsion is five dripping stages; the dripping sequence of the five dripping stages includes a first dripping stage, a first pause stage, a second dripping stage, a second pause stage, a third dripping stage, a third pause stage, a fourth dripping stage, a fourth pause stage, and a fifth dripping stage; the dripping time of the first dripping stage is 31 min, the dripping amount of the first dripping stage is 77.5 wt% of component C, the pause time of the first pause stage is 9 min, and the dripping time of the second dripping stage is 10 min. The dripping time of the second dripping stage is 1min, the dripping amount of the second dripping stage is 2.5wt% of component C, the pause time of the second pause stage is 6min, the dripping time of the third dripping stage is 1min, the dripping amount of the third dripping stage is 2.5wt% of component C, the pause time of the third pause stage is 3min, the dripping time of the fourth dripping stage is 2min, the dripping amount of the fourth dripping stage is 5wt% of component C, the pause time of the fourth pause stage is 5min, the dripping time of the fifth dripping stage is 5min, and the dripping amount of the fourth dripping stage is the remainder component C.
[0249] The temperature for heat preservation in S3 is 17.4° C., the stirring speed during heat preservation in S3 is 293 r / min, and the heat preservation time is 90 min.
[0250] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0251] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0252] Embodiment 14
[0253] The first aspect of this embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole. The specific implementation method is the same as that of Example 13, except that:
[0254] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 18.4°C.
[0255] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 361 r / min.
[0256] The emulsion in S3 is dripped with component C at a stirring speed of 361r / min, and the dripping stage of component C dripping into the emulsion is five dripping stages; the dripping sequence of the five dripping stages includes a first dripping stage, a first pause stage, a second dripping stage, a second pause stage, a third dripping stage, a third pause stage, a fourth dripping stage, a fourth pause stage, and a fifth dripping stage; the dripping time of the first dripping stage is 31min, the dripping amount of the first dripping stage is 77.5wt% of component C, the pause time of the first pause stage is 9min, and the dripping time of the second dripping stage is 10min. The dripping time of the second dripping stage is 1min, the dripping amount of the second dripping stage is 2.5wt% of component C, the pause time of the second pause stage is 6min, the dripping time of the third dripping stage is 1min, the dripping amount of the third dripping stage is 2.5wt% of component C, the pause time of the third pause stage is 3min, the dripping time of the fourth dripping stage is 2min, the dripping amount of the fourth dripping stage is 5wt% of component C, the pause time of the fourth pause stage is 5min, the dripping time of the fifth dripping stage is 5min, and the dripping amount of the fourth dripping stage is the remainder component C.
[0257] The temperature for heat preservation in S3 is 18.4° C., the stirring speed during heat preservation in S3 is 361 r / min, and the heat preservation time is 90 min.
[0258] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0259] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0260] The sixth experiment
[0261] The sixth group of experiments includes Example 15, Example 16, Example 17, and Example 18.
[0262] Embodiment 15
[0263] The first aspect of the present embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0264] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0265] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0266] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0267] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0268] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0269] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0270] The specific names and amounts of raw materials used are shown in Table 2.
[0271] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 15°C.
[0272] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 400 r / min.
[0273] The emulsion in S3 is dripped with component C at a stirring speed of 400 r / min, and the dripping stage of component C into the emulsion is a single dripping stage; the dripping time of the single dripping stage is 30 min, and the dripping amount of the single dripping is 100 wt% of component C.
[0274] The temperature for heat preservation in S3 is 15° C., the stirring speed during heat preservation in S3 is 400 r / min, and the heat preservation time is 90 min.
[0275] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0276] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0277] Example 16
[0278] The first aspect of this embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of Example 15, except that:
[0279] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 30°C.
[0280] The temperature for heat preservation in S3 is 30° C., the stirring speed during heat preservation in S3 is 400 r / min, and the heat preservation time is 90 min.
[0281] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0282] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0283] Embodiment 17
[0284] The first aspect of this embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of Example 15, except that:
[0285] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 40°C.
[0286] The temperature for heat preservation in S3 is 40° C., the stirring speed during heat preservation in S3 is 400 r / min, and the heat preservation time is 90 min.
[0287] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0288] The third aspect of this embodiment provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0289] Embodiment 18
[0290] The first aspect of this embodiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of Example 15, except that:
[0291] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 50°C.
[0292] The temperature for heat preservation in S3 is 50° C., the stirring speed during heat preservation in S3 is 400 r / min, and the heat preservation time is 90 min.
[0293] The seventh experiment
[0294] The seventh group of experiments includes Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4.
[0295] Comparative Example 1
[0296] The first aspect of the present comparative example provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0297] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0298] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0299] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added for modulation to obtain a microcapsule suspension containing benzylpyridamole.
[0300] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0301] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0302] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0303] The specific names and amounts of raw materials used are shown in Table 2.
[0304] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 18.4°C.
[0305] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 251 r / min.
[0306] The emulsion in S3 is added with component C at a stirring speed of 251r / min, and the dropping stage of component C into the emulsion is a single dropping stage; the dropping time of the single dropping stage is 10min, and the dropping amount of the single dropping is 100wt% of component C. The problem of violent aggregation has occurred during the dropping process; component D is not added for subsequent modulation.
[0307] Comparative Example 2
[0308] The first aspect of this comparative example provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of comparative example 1, except that:
[0309] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 19.6°C.
[0310] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 292 r / min.
[0311] The emulsion in S3 is added with component C at a stirring speed of 292 r / min, and the dropping stage of component C into the emulsion is a single dropping stage; the dropping time of the single dropping stage is 10 min, and the dropping amount of the single dropping is 100 wt% of component C. Agglomeration problem has occurred during the dropping process; component D is not added for modulation subsequently.
[0312] Comparative Example 3
[0313] The first aspect of the present comparative example provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0314] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0315] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0316] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0317] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0318] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0319] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0320] The specific names and amounts of raw materials used are shown in Table 2.
[0321] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 21.9°C.
[0322] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 400 r / min.
[0323] The emulsion in S3 is added with component C at a stirring speed of 400 r / min, and the dropping stage of component C into the emulsion is a single dropping stage; the dropping time of the single dropping stage is 20 min, and the dropping amount of the single dropping is 95wt% of component C. After that, the problem of sudden polymerization occurs, and the remaining component C is not continued to be dropped, and component D is not added for subsequent modulation.
[0324] Comparative Example 4
[0325] The first aspect of this comparative example provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of comparative example 3, except that:
[0326] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 23.5°C.
[0327] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 400 r / min.
[0328] The emulsion in S3 is added with component C at a stirring speed of 400 r / min, and the dropping stage of component C into the emulsion is a single dropping stage; the dropping time of the single dropping stage is 20 min, and the dropping amount of the single dropping is 95wt% of component C. After that, the problem of sudden polymerization occurs, and the remaining component C is not continued to be dropped, and component D is not added for subsequent modulation.
[0329] The eighth experiment
[0330] The eighth group of experiments includes Comparative Example 5 and Comparative Example 6.
[0331] Comparative Example 5
[0332] The first aspect of the present comparative example provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0333] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0334] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0335] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0336] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0337] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0338] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0339] The specific names and amounts of raw materials used are shown in Table 2.
[0340] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 18°C.
[0341] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 293 r / min.
[0342] The emulsion in S3 is dripped with component C at a stirring speed of 293r / min, and the dripping stage of component C into the emulsion is a secondary dripping stage; the dripping sequence of the secondary dripping stage includes a first dripping stage, a first pause stage, and a second dripping stage; the dripping time of the first dripping stage is 14min, the dripping amount of the first dripping stage is 50wt% of component C, the pause time of the first pause stage is 52min, the dripping time of the second dripping stage is 28min, and the dripping amount of the second dripping stage is the remaining component C.
[0343] The temperature for heat preservation in S3 is 18° C., the stirring speed during heat preservation in S3 is 293 r / min, and the heat preservation time is 90 min.
[0344] The second aspect of this embodiment provides a microcapsule suspension containing benzylpyridazine, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridazine as described above.
[0345] Comparative Example 6
[0346] The first aspect of this comparative example provides a method for preparing a microcapsule suspension containing benzylpyridamole, and the specific implementation method is the same as that of comparative example 5, except that:
[0347] In S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 25°C.
[0348] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 416 r / min.
[0349] The emulsion in S3 is dripped with component C at a stirring speed of 416 r / min, and the dripping stage of component C being dripped into the emulsion is a secondary dripping stage; the dripping sequence of the secondary dripping stage includes a first dripping stage, a first pause stage, and a second dripping stage; the dripping time of the first dripping stage is 14 min, the dripping amount of the first dripping stage is 50 wt% of component C, the pause time of the first pause stage is 52 min, the dripping time of the second dripping stage is 28 min, and the dripping amount of the second dripping stage is the remaining component C.
[0350] The temperature for heat preservation in S3 is 25° C., the stirring speed during heat preservation in S3 is 416 r / min, and the heat preservation time is 90 min.
[0351] The ninth experiment
[0352] The ninth set of experiments includes Examples 19 to 25.
[0353] The ninth group of experiments provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0354] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0355] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0356] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0357] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0358] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0359] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0360] The specific names and amounts of raw materials used are shown in Table 2.
[0361] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 19.4°C.
[0362] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 293 r / min.
[0363] The emulsion in S3 is dripped with component C at a stirring speed of 293 r / min, and the dripping stage of component C into the emulsion is a single dripping stage; the dripping time of the single dripping stage is 30 min, and the dripping amount of the single dripping is 100 wt% of component C.
[0364] The temperature for heat preservation in S3 is 19.4° C., the stirring speed during heat preservation in S3 is 293 r / min, and the heat preservation time is 90 min.
[0365] The amounts of raw materials used in Examples 19-24 in the ninth group of experiments are shown in Table 4.
[0366] Table 4
[0367]
[0368]
[0369] The amounts of raw materials used in Example 25 are shown in Table 5.
[0370] Table 5
[0371]
[0372] The second aspect of the ninth group of experiments provides a microcapsule suspension containing benzylpyridamole, which is prepared by the preparation method of the microcapsule suspension containing benzylpyridamole as described above.
[0373] The third aspect of the ninth group of experiments provides an application of a microcapsule suspension containing benzylpyridamole, which is applied in the field of weed control technology.
[0374] The tenth experiment
[0375] The tenth set of experiments included Example 26.
[0376] The tenth group of experiments provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0377] S1. The benzylpyridamole, solvent, oil-soluble capsule material and emulsifier are mixed uniformly to form component A;
[0378] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0379] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0380] The component B is formed by uniformly mixing a dispersant, a defoamer and water.
[0381] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0382] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0383] The specific names and amounts of raw materials used are shown in Table 2.
[0384] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 19.4°C.
[0385] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 293 r / min.
[0386] The emulsion in S3 is dripped with component C at a stirring speed of 293 r / min, and the dripping stage of component C into the emulsion is a single dripping stage; the dripping time of the single dripping stage is 30 min, and the dripping amount of the single dripping is 100 wt% of component C.
[0387] The temperature for heat preservation in S3 is 19.4° C., the stirring speed during heat preservation in S3 is 293 r / min, and the heat preservation time is 90 min.
[0388] The amounts of raw materials used in Example 26 in the ninth group of experiments are shown in Table 6.
[0389] Table 6
[0390]
[0391]
[0392] Experiment 11
[0393] The eleventh experiment includes Comparative Examples 7 to 13.
[0394] The eleventh experiment provides a method for preparing a microcapsule suspension containing benzylpyridamole, comprising the following steps:
[0395] S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A;
[0396] S2. Adding component A to component B and stirring and shearing to form an emulsion;
[0397] S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added after heat preservation to obtain a microcapsule suspension containing benzylpyridamole.
[0398] The component B is formed by uniformly mixing an emulsifier, a dispersant, a defoamer and water.
[0399] The component C is formed by uniformly mixing a water-soluble capsule material and water.
[0400] The component D is formed by uniformly mixing a dispersant, a structure regulator, an antifreeze agent and a preservative.
[0401] In the step S3, the temperature at which component C is added dropwise to the emulsion for reaction is controlled to be 19.4°C.
[0402] In the S2, the stirring speed of adding component A into component B for stirring and shearing is 293 r / min.
[0403] The emulsion in S3 is dripped with component C at a stirring speed of 293 r / min, and the dripping stage of component C into the emulsion is a single dripping stage; the dripping time of the single dripping stage is 30 min, and the dripping amount of the single dripping is 100 wt% of component C.
[0404] The temperature for heat preservation in S3 is 19.4° C., the stirring speed during heat preservation in S3 is 293 r / min, and the heat preservation time is 90 min.
[0405] The amounts of raw materials used in Comparative Examples 7-13 in the eleventh group of experiments are shown in Table 7.
[0406] Table 7
[0407]
[0408]
[0409] Performance Testing
[0410] 1. Preparation process stability test:
[0411] Whether the phenomenon of sudden aggregation and creaming occurs in the process of preparing the microcapsule suspension containing benzylpyridamole in the first to eleventh experiments is recorded. The test results are shown in Table 8.
[0412] 2. Hot or cold storage stability test:
[0413] The microcapsule suspension containing benzylpyrimidine provided in the embodiment that does not have the phenomenon of sudden aggregation and creaming in the process of preparing the microcapsule suspension containing benzylpyrimidine in the first group of experiments to the eleventh group of experiments is subjected to hot storage and cold storage respectively. The hot storage condition is: hot storage for 14 days, the hot storage temperature is (54±2)℃, and a microscope is used to observe whether the microcapsule suspension containing benzylpyrimidine will have adhesion after 14 days of hot storage. The test results are shown in Table 7; the cold storage condition is: cold storage at -25℃ for 24h, then taken out and placed at room temperature for 24h, and then cold storage at -25℃ again, and the cycle is repeated 7 times, and the physical stability of the system is observed. The morphological changes of the microcapsules after storage are observed under a microscope. The test results are shown in Table 9.
[0414] The microscope was used for observation at a magnification of 400 times.
[0415] After hot storage, the microscope was used to observe that there was no aggregation and adhesion. Figure 1 .
[0416] After hot storage, microscopic observation showed that agglomeration and adhesion problems had occurred, and there was a state of violent aggregation. Figure 2 .
[0417] After cold storage, microscopic observation showed that the problem of agglomeration and adhesion had occurred, and the problem of violent aggregation was seen. Figure 3 .
[0418] The state of sudden aggregation problem during the preparation process is shown in Figure 4 .
[0419] See the sample bottles used for hot storage. Figure 5 .
[0420] Sample bottles used for cold storage are shown in Figure 6 .
[0421] 3. pH change state test:
[0422] In the sixth group of experiments, the pH value of the microcapsule suspension system changes with the insulation time when different temperatures are used for insulation in Test Example 15, Example 16, Example 17 and Example 18. The test results are shown in Table 10. Table 10 shows the pH value of the test microcapsule suspension system when the insulation time is 0 min, 10 min, 20 min, 30 min, 40 min, 50 min, 60 min, 70 min, 80 min and 90 min, respectively.
[0423] Table 8
[0424]
[0425]
[0426] Table 9
[0427] Example Preparation process stability test Thermal storage stability test Cold storage stability test Comparative Example 1 A violent gathering Failed, not tracked Failed, not tracked Comparative Example 2 A violent gathering Failed, not tracked Failed, not tracked Comparative Example 3 A violent gathering Failed, not tracked Failed, not tracked Comparative Example 4 A violent gathering Failed, not tracked Failed, not tracked Comparative Example 5 No violent aggregation, no paste There is agglomeration and adhesion phenomenon There is agglomeration and adhesion phenomenon Comparative Example 6 No violent aggregation, no paste There is agglomeration and adhesion phenomenon There is agglomeration and adhesion phenomenon Comparative Example 7 There is violent aggregation and paste Failed, not tracked Failed, not tracked Comparative Example 8 There is violent aggregation and paste Failed, not tracked Failed, not tracked Comparative Example 9 A violent gathering Failed, not tracked Failed, not tracked Comparative Example 10 There is violent aggregation and paste Failed, not tracked Failed, not tracked Comparative Example 11 A violent gathering Failed, not tracked Failed, not tracked Comparative Example 12 A violent gathering Failed, not tracked Failed, not tracked Comparative Example 13 No violent aggregation, no paste Thermal storage curing Failed, not tracked
[0428] It can be seen from the above test results that when a phosphate dispersant and a hydrophilic modified copolymer carboxylate dispersant are used in combination, the problem of violent aggregation will easily occur when component C is added dropwise into the emulsion for solidification into capsules. When a hydrophilic modified copolymer carboxylate dispersant is used to replace the dispersant obtained by compounding a phosphate dispersant and a hydrophilic modified copolymer carboxylate dispersant, the problem of violent aggregation that will easily occur during solidification into capsules can be solved.
[0429] It can be seen from the above test results that when the mass ratio of oil-soluble capsule material to water-soluble capsule material is 6:1, the problem of component C being prone to reaction and polymerization when it is added dropwise into the emulsion for solidification into capsules can be improved.
[0430] Table 10
[0431]
[0432]
[0433] Table 10 shows the change in pH value in the emulsion after Example 15 in the sixth group of experiments in which component C is added dropwise to the emulsion for reaction at 15°C, in Example 16 in which component C is added dropwise to the emulsion for reaction at 30°C, in Example 17 in which component C is added dropwise to the emulsion for reaction at 40°C, and in Example 18 in which component C is added dropwise to the emulsion for reaction at 50°C.
Claims
1. A method for preparing a microcapsule suspension containing benzylpyridamole, characterized in that: The following steps are involved: S1. The benzylpyridamole, solvent, and oil-soluble capsule material are mixed uniformly to form component A; S2. Adding component A to component B and stirring and shearing to form an emulsion; S3. Component C is added dropwise to the emulsion to react and solidify into capsules, and then component D is added for modulation after heat preservation to obtain a microcapsule suspension containing benzylpyridamole; The component B includes one or more combinations of emulsifier, dispersant, defoamer and water; The component C comprises one or a combination of water-soluble capsule material and water; The component D comprises a combination of one or more of a dispersant, a structure regulator, an antifreeze agent, and a preservative; In S3, the temperature of adding component C dropwise into the emulsion for reaction is controlled to be ≤40°C.
2. The method for preparing the microcapsule suspension containing benzylpyridamole as claimed in claim 1, characterized in that: In the S2, the stirring speed of adding component A into component B for stirring and shearing is 290-465 r / min.
3. The method for preparing the microcapsule suspension containing benzylpyridamole as claimed in claim 1, characterized in that: In the S3, component C is added dropwise to the emulsion at a stirring speed of 290-465 r / min, and the dropping stage of component C into the emulsion includes at least one dropping stage.
4. The method for preparing the microcapsule suspension containing benzylpyridamole as claimed in claim 3, characterized in that: The dropping time in the dropping stage in S3 is 30-90 min.
5. The method for preparing the microcapsule suspension containing benzylpyridamole according to any one of claims 1 to 4, characterized in that: The time required to pause during the process of adding component C dropwise to the emulsion in S3 is 0-30 minutes.
6. The method for preparing the microcapsule suspension containing benzylpyridamole as claimed in claim 3, characterized in that: The step of adding component C dropwise to the emulsion in S3 includes one dropping step, two dropping steps, three dropping steps, four dropping steps, or five dropping steps.
7. The method for preparing the microcapsule suspension containing benzylpyridamole as claimed in claim 6, characterized in that: The dripping time of the single dripping stage is 30-90 minutes, and the dripping amount of the single dripping is 100 wt% of component C.
8. The method for preparing the microcapsule suspension containing benzylpyridamole as claimed in claim 6, characterized in that: The dropping sequence of the secondary dropping stage includes a first dropping stage, a first pause stage, and a second dropping stage; the dropping time of the first dropping stage is 20-25 minutes, the dropping amount of the first dropping stage is 50-65wt% of component C, the pause time of the first pause stage is 4-10 minutes, the dropping time of the second dropping stage is 10-15 minutes, and the dropping amount of the second dropping stage is the remaining component C.
9. The method for preparing the microcapsule suspension containing benzylpyridamole as claimed in claim 6, characterized in that: The dropping sequence of the three dropping stages includes a first dropping stage, a first pause stage, a second dropping stage, a second pause stage, and a third dropping stage; the dropping time of the first dropping stage is 25-35min, the dropping amount of the first dropping stage is 70-75wt% of component C, the pause time of the first pause stage is 3-8min, the dropping time of the second dropping stage is 5-10min, the dropping amount of the second dropping stage is 12-20wt% of component C, the pause time of the second pause stage is 3-8min, the dropping time of the third dropping stage is 3-8min, and the dropping amount of the third dropping stage is the remainder component C.
10. The method for preparing the microcapsule suspension containing benzylpyridamole according to claim 6, characterized in that: The dropping sequence of the four dropping stages includes a first dropping stage, a first pause stage, a second dropping stage, a second pause stage, a third dropping stage, a third pause stage, and a fourth dropping stage; the dropping time of the first dropping stage is 20-30 min, the dropping amount of the first dropping stage is 55-63wt% of component C, the pause time of the first pause stage is 3-8 min, the dropping time of the second dropping stage is 5-10 min, the dropping amount of the second dropping stage is 15-24wt% of component C, the pause time of the second pause stage is 3-8 min, the dropping time of the third dropping stage is 1-8 min, the dropping amount of the third dropping stage is 6-12wt% of component C, the pause time of the third pause stage is 1-8 min, the dropping time of the fourth dropping stage is 1-8 min, and the dropping amount of the fourth dropping stage is the remainder component C.
11. The method for preparing the microcapsule suspension containing benzylpyridamole according to claim 6, characterized in that: The order of the five dropping stages includes a first dropping stage, a first pause stage, a second dropping stage, a second pause stage, a third dropping stage, a third pause stage, a fourth dropping stage, a fourth pause stage, and a fifth dropping stage; the dropping time of the first dropping stage is 28-35min, the dropping amount of the first dropping stage is 75-80wt% of component C, the pause time of the first pause stage is 6-12min, the dropping time of the second dropping stage is 0.5-3min, the dropping amount of the second dropping stage is 1-5wt% of component C, and the The pause time of the second pause stage is 3-8min, the dropping time of the third dropping stage is 0.5-3min, the dropping amount of the third dropping stage is 1-5wt% of component C, the pause time of the third pause stage is 1-5min, the dropping time of the fourth dropping stage is 0.5-4min, the dropping amount of the fourth dropping stage is 2-8wt% of component C, the pause time of the fourth pause stage is 1-8min, the dropping time of the fifth dropping stage is 1-8min, and the dropping amount of the fourth dropping stage is the remainder component C.
12. A microcapsule suspension containing benzylpyridamole, characterized in that: The microcapsule suspension containing benzylpyridamole is prepared by the preparation method according to any one of claims 1 to 11.
13. A use of the microcapsule suspension containing benzylpyridamole as claimed in claim 12, characterized in that: Used in the field of weed control technology.
Citation Information
Patent Citations
Microcapsule suspending agent for pesticides as well as preparation method and application of microcapsule suspending agent
CN108432751A