CN114762502A - Acaricide suspending agent and preparation thereof - Google Patents
Acaricide suspending agent and preparation thereof Download PDFInfo
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- CN114762502A CN114762502A CN202110041401.1A CN202110041401A CN114762502A CN 114762502 A CN114762502 A CN 114762502A CN 202110041401 A CN202110041401 A CN 202110041401A CN 114762502 A CN114762502 A CN 114762502A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having no bond to a nitrogen atom
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
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- A01N41/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom
- A01N41/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom containing a sulfur-to-oxygen double bond
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- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
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Abstract
The invention belongs to the field of pesticide acaricide, and relates to an acaricide suspending agent and a preparation method thereof. The acaricide suspending agent comprises an effective active ingredient and an auxiliary agent, wherein the effective active ingredient is a compound with acaricidal activity, the auxiliary agent in the suspending agent contains a suspending substance, the addition amount of the suspending substance accounts for 0.01-10% of the weight of the acaricide suspending agent, and the suspending substance is xanthan gum and/or polyvinyl alcohol. By adopting the method of the invention, the suspending agent with high suspension rate and excellent drug effect can be obtained.
Description
Technical Field
The invention belongs to the field of pesticide acaricide, and relates to an acaricide suspending agent and preparation thereof.
Background
The first ten market shares of the Chinese acaricide account for 70 percent of the total market share. The first five crops in the application field of the Chinese acaricide are respectively orange, apple, vegetable, cotton and potato. The largest application crop field is citrus, which accounts for 52% of the total acaricide market share. The application of acaricides plays a key role in the growth of crops. The current acaricide comprises pyraclostrobin (SYP-9625), spirotetramat, etoxazole, spirodiclofen, propargite, bifenazate, pyridaben, abamectin, hexythiazox, flutriafol and the like.
The compound with acaricidal activity is expected to really exert efficacy, and an applicable formulation is necessarily required to be endowed by virtue of pesticide formulation technology, but the technology for preparing the compound into the applicable formulation is already popularized at present, but key performances in the formulation are still researched and strengthened, such as the improvement of formulation stability, the control of formulation particle size, the improvement of suspension performance of the formulation and the like, and the final aim of the improvement of the performances is to better exert the biological activity of the compound. The suspension property of the pesticide preparation is one of the most important indexes influencing the activity of the compound, because the compound is diluted into liquid medicine to be sprayed to exert the pesticide effect after being prepared into the preparation. The suspension property is just the embodiment of the uniformity and the effectiveness of the diluted liquid medicine. The related standards of the current pesticide industry include that the suspension rate of a plurality of product standards is required to be greater than or equal to 90%, and the data is a threshold value, and in research, the micro improvement of the pesticide effect is found to greatly improve the pesticide effect especially for the current acaricide with serious resistance, so that the improvement of the suspension performance, such as the improvement of the suspension rate from greater than or equal to 90% to greater than or equal to 98%, is a very significant progress.
In the relevant documents and technical data, the improvement of the suspension performance is basically realized by adopting a means of a surfactant in the pesticide preparation, and the suspension rate can be controlled to be more than 90%. However, the suspension rate of the acaricide is required to reach more than 98%, and the suspending substance and the corresponding process discovered by the invention are not used for overcoming and solving the problem in the prior art.
Disclosure of Invention
The invention aims to provide an acaricide suspending agent and preparation thereof.
In order to realize the purpose, the technical scheme of the invention is as follows:
the suspending agent comprises an effective active ingredient and an auxiliary agent, wherein the effective active ingredient is a compound with acaricidal activity, the auxiliary agent in the suspending agent contains a suspending substance, the addition amount of the suspending substance accounts for 0.01-10% of the weight of the suspending agent, and the suspending substance is xanthan gum and/or polyvinyl alcohol.
The addition amount of the xanthan gum accounts for 0.01-0.3% of the weight of the preparation; the addition amount of the polyvinyl alcohol accounts for 1 to 5 percent of the weight of the preparation.
The effective active ingredients are selected from one or more of ethacrylonitrile, spirotetramat and a compound A; wherein, the structural formula of the compound A is as follows:
the effective active ingredients of the suspending agent account for 5-60% of the weight of the preparation.
A method for preparing acaricide suspending agent comprises mixing and dispersing other components except suspending agent uniformly according to a certain proportion, sanding until the particle diameter D50 is less than 2 microns to obtain liquid medicine stock solution, then adding suspending agent xanthan gum into the liquid medicine stock solution in a mixing and stirring manner according to a certain proportion, adding polyvinyl alcohol after uniformly mixing, and dispersing uniformly to obtain the acaricide suspending agent.
The suspending agent is prepared according to the method, the active components can be selected from the group consisting of ethacrylonitrile, spirotetramat and the compound A, and the technical scheme can also be applied to other acaricides to improve the suspension performance, so that the excellent control effect is obtained.
In addition, the auxiliary agent used in the suspending agent system can adopt the auxiliary agent which is conventionally used in the suspending agent system, such as wetting dispersant, the addition amount is 2-30%, and the auxiliary agent can be selected from one or more of lignosulfonate, macromolecular carboxylate, naphthalenesulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfonate, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and macromolecular amphiphilic anionic and nonionic compound surfactant; the emulsifier is added in an amount of 2-20%, and can be selected from one or more of anionic surfactant, nonionic surfactant and anionic and nonionic compound surfactant; wherein the anionic surfactant mainly comprises calcium dodecylbenzene sulfonate and sodium polyacrylate; the nonionic surfactant is mainly castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether, phenethyl phenol polyoxyethylene ether, alkylphenol polyoxyethylene formaldehyde condensate, fatty alcohol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, styrene maleic anhydride copolymer, phenethyl phenol polyoxyethylene polyoxypropylene ether and formaldehyde condensate.
The invention has the advantages that:
in the suspending agent, xanthan gum which is used as a conventional suspending agent and has the thickening and stabilizing effects acts on suspending substances of the suspending agent, the suspending substances are mixed with other components of the suspending agent and then subjected to sanding, and the suspending substances are added in a dispersing and stirring manner at a specific time after sanding is finished, so that the effect of obviously improving the suspension rate can be achieved. Meanwhile, the suspending agent can be mixed with polyvinyl alcohol according to a special process to prepare the suspending agent, so that the problem of poor suspension performance of a suspension system can be effectively solved, the suspension performance of the liquid medicine is improved, the drug effect of the preparation can be improved, and the synergistic effect is achieved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, but the present invention is by no means limited to these examples. The embodiments of the present invention, and all other embodiments obtained by a person of ordinary skill in the art without any inventive work, belong to the scope of protection of the present invention. The percentages in the formulation are by weight. Ethizole acarbonitrile (Shenyang scientific chemical product Co., Ltd., content 98%), spirotetramat (Bayer corporation, content 98%), and compound A (Shenyang chemical pesticide chemical research and development Co., Ltd., Chinese invention patent CN 105541682A, preparation method, content 98.5%) were added after being folded into hundreds, and other raw materials were all commercial products.
The prepared suspending agent can be diluted by a user or directly sprayed with water before use, and can also be directly used.
Formulation examples of formulations
Example 1, 20% Chlorobipyr-spirotetramat suspension
According to the formula requirements, the fluxapyroxad is treated according to the two process methods of (1) and (2) respectively, wherein the fluxapyroxad is 10%, the spirotetramat is 10%, the Atlox is 49135%, the SK 242% and the deionized water is 23%.
(1) The materials are sequentially added into a mixing tank to be mixed, 0.15 percent of xanthan gum, 2 percent of polyvinyl alcohol and deionized water are continuously added to complement to 100 percent. Firstly, dispersing and mixing in a coarse step, then transferring into a sand mill for sand milling, detecting the granularity of the sand milled material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 micrometers to obtain liquid medicine A.
(2) The preparation method comprises the steps of sequentially adding the substances into a mixing tank for mixing, dispersing and mixing through a coarse step, then transferring into a sand mill for sand milling, detecting the granularity of a sand-milled material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 micrometers to obtain liquid medicine A. And dispersing and stirring the liquid medicine A, keeping the rotating speed to be more than 20rpm, adding 0.15% of xanthan gum, 2% of polyvinyl alcohol and 100% of deionized water under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The preparation formulas and the processes of the (1) and (2) are respectively used for two comparative tests with no addition of polyvinyl alcohol or no addition of xanthan gum and polyvinyl alcohol; the suspending agent suspension data were identical for both methods when no xanthan gum and polyvinyl alcohol were added.
Respectively measuring the suspension performance and the suspension rate of the prepared 20% ethiprole-spirotetramat suspension:
determination of suspension Properties: weighing 5g of a sample, dropwise adding the sample into a 100mL measuring cylinder, standing for 24h, measuring and recording the precipitation condition at the bottom of the measuring cylinder, wherein the less the precipitation, the better the suspension performance.
And (3) suspension rate determination: sample 1g (to the nearest 0.0002g) was weighed and assayed at 4.5 in GB/T14825-2006. The remaining 25mL of suspension and precipitate were washed with 45mL of acetonitrile three times, transferred into a 50mL volumetric flask, ultrasonically shaken for 10min, returned to room temperature, made to volume with acetonitrile, and shaken up. And (3) taking part of the test solution in a centrifuge tube, carrying out centrifugal separation, taking supernatant, and calculating the suspension rate according to the mass of the effective components.
The subsequent parts related to the determination of the suspension property and the suspension rate adopt the method.
Table 120% ethacrylonitrile-spirotetramat suspension data
According to the formula requirements, the amount of the suspending agent is increased according to the process procedures of (1) and (2), if the amount of the xanthan gum is 0.32%, the polyvinyl alcohol is 5.5%, and the deionized water is used for supplementing 100%, the system is completely viscous and creamy, and 20% of the ethiprole-spirotetramat suspending agent cannot be normally prepared.
Example 2, 30% Etoxazole Acanthonitrile spirotetramat suspension
According to the formula requirements, 15% of ethazoxazole nitrile, 15% of spirotetramat, 49135% of Atlox, 34 SK34SC 2 and 13% of deionized water are respectively treated according to the two process methods of (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.15 percent of xanthan gum, 2 percent of polyvinyl alcohol and deionized water are continuously added to be complemented to 100 percent. The preparation method comprises the steps of firstly dispersing and mixing in a coarse step, then transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 microns to obtain the liquid medicine B. (2) Adding the above-mentioned substances into the blending tank in proper order and mixing, firstly through coarse step dispersion mixing, then transferring into the sand mill and carrying out the sanding, detect the granularity of sanding material with the particle size distribution appearance, after particle diameter D50 is less than or equal to 2 microns, filter, obtain liquid medicine B. And (3) dispersing and stirring the liquid medicine B, keeping the rotating speed to be more than 20rpm, adding 0.15% of xanthan gum, 2% of polyvinyl alcohol and 100% of deionized water to complement under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The preparation formula and the process of the above (1) and (2) are carried out, and only xanthan gum is added as a comparative test.
And respectively measuring the suspension performance and the suspension rate of the prepared 30% ethiprole-spirotetramat suspension.
TABLE 230% Chlorobipyr-spirotetramat suspending agent suspension data
According to the formula requirements, according to the processes of (1) and (2), if the amount of xanthan gum is 0.35%, the polyvinyl alcohol is 5.1% and the deionized water is added to 100%, the system is completely viscous and creamed, and the 30% ethacrylonitrile-spirotetramat suspending agent cannot be normally prepared.
Example 3, 35% Chlorobipyr-spirotetramat suspension
According to the formula requirements, 30% of ethaboxam, 5% of spirotetramat, 6% of TENSILOX DB 086%, 243% of SK and 6% of deionized water are respectively treated according to the two process methods (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.05 percent of xanthan gum, 1 percent of polyvinyl alcohol and deionized water are continuously added to complement to 100 percent. The preparation method comprises the steps of firstly carrying out coarse-step dispersing and mixing, then transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 microns to obtain the liquid medicine C. (2) Adding the above materials into a mixing tank in sequence for mixing, performing coarse step dispersion mixing, transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering to obtain liquid medicine C when the particle size D50 is less than or equal to 2 micrometers. And (3) dispersing and stirring the liquid medicine C, keeping the rotating speed to be more than 20rpm, adding 0.05% of xanthan gum, 1% of polyvinyl alcohol and deionized water to complement 100% under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The preparation formula and the process of the above (1) and (2) are carried out, and only xanthan gum is added as a comparative test.
And respectively measuring the suspension performance and the suspension rate of the prepared 35% ethacrylonitrile-spirotetramat suspension.
TABLE 335% Chlorobipyr and spirotetramat suspending agent suspension data
Example 4, 40% Chlorobipyr-spirotetramat suspension
According to the formula requirements, 20% of ethaboxam, 20% of spirotetramat, 30006% of YUS-FS, 243% of SK and 11% of deionized water are respectively treated according to the two process methods (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.01 percent of xanthan gum, 5 percent of polyvinyl alcohol and deionized water are continuously added to complement to 100 percent. The preparation method comprises the steps of firstly dispersing and mixing in a coarse step, then transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 microns to obtain the liquid medicine D. (2) Adding the above-mentioned material into blending tank in proper order and mixing, firstly through the coarse step dispersion mixing, then transferring into the sand mill and carrying out the sanding, detect the granularity of sanding material with the particle size distribution appearance, after particle diameter D50 is less than or equal to 2 microns, filter, obtain liquid medicine D. And (3) dispersing and stirring the liquid medicine D, keeping the rotating speed to be more than 20rpm, adding 0.01% of xanthan gum, 5% of polyvinyl alcohol and 100% of deionized water to complement under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The above formula and process of (1) and (2) are prepared, and xanthan gum is added only as a comparison test.
And respectively measuring the suspension performance and the suspension rate of the prepared 40% ethiprole-spirotetramat suspension.
TABLE 440% Chlorobipyr-spirotetramat suspending agent suspension data
Example 5, 15% Compound A suspension
According to the formula requirements, compound A15%, Atlox 49162%, NNO 3% and deionized water 30% are respectively treated according to the two process methods (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.3 percent of xanthan gum, 1 percent of polyvinyl alcohol and deionized water are continuously added to complement to 100 percent. The preparation method comprises the steps of firstly carrying out coarse-step dispersing and mixing, then transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 microns to obtain the liquid medicine E. (2) Adding the above materials into a mixing tank in sequence for mixing, performing coarse step dispersion mixing, transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering to obtain liquid medicine E when the particle size D50 is less than or equal to 2 micrometers. And (3) dispersing and stirring the liquid medicine E, keeping the rotating speed to be more than 20rpm, adding 0.3% of xanthan gum, 1% of polyvinyl alcohol and deionized water to complement 100% under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The preparation formulas and the processes of the (1) and (2) are respectively used for two comparative tests with no addition of polyvinyl alcohol or no addition of xanthan gum and polyvinyl alcohol; the suspending agent suspension data for both methods were identical when xanthan gum and polyvinyl alcohol were not added simultaneously.
The suspension performance and the suspension rate of the prepared 15% compound A suspension agent are respectively measured.
Table 515% compound a suspending agent suspension data
Example 6, 20% Compound A suspending agent
According to the formula requirements, 20% of compound A, 49133% of Atlox, 1% of NNO and 26% of deionized water are respectively treated according to the two process methods (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.25 percent of xanthan gum, 2 percent of polyvinyl alcohol and deionized water are continuously added to be complemented to 100 percent. Firstly, coarse-step dispersion and mixing are carried out, then the mixture is transferred into a sand mill for sand milling, the granularity of the sand-milled material is detected by a granularity distribution instrument, and after the grain diameter D50 is less than or equal to 2 micrometers, the mixture is filtered to obtain liquid medicine F. (2) The preparation method comprises the steps of sequentially adding the substances into a mixing tank for mixing, dispersing and mixing through a coarse step, then transferring into a sand mill for sand milling, detecting the granularity of a sand-milled material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 micrometers to obtain liquid medicine F. And (3) dispersing and stirring the liquid medicine F, keeping the rotating speed to be more than 20rpm, adding 0.25% of xanthan gum, 2% of polyvinyl alcohol and deionized water to complement 100% under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The above formula and process of (1) and (2) are prepared, and xanthan gum is added only as a comparison test.
The suspension performance and the suspension rate of the prepared 20% compound A suspension agent are respectively measured.
Table 620% compound a suspending agent suspension data
Example 7, 30% Compound A suspending agent
According to the formula requirements, 30% of compound A, GY-D072%, SP 27282% and 16% of deionized water are respectively treated according to the two process methods (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.05 percent of xanthan gum, 3 percent of polyvinyl alcohol and deionized water are continuously added to complement to 100 percent. Firstly, dispersing and mixing in a coarse step, then transferring into a sand mill for sand milling, detecting the granularity of the sand milled material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 micrometers to obtain liquid medicine G. (2) Adding the above-mentioned material in proper order into the blending tank and mixing, earlier through coarse step dispersion mixing, then transferring into the sand mill and carrying out the sanding, detect the granularity of sanding material with the particle size distribution appearance, after particle diameter D50 is less than or equal to 2 microns, filter, obtain liquid medicine G. And (3) dispersing and stirring the liquid medicine G, keeping the rotating speed to be more than 20rpm, adding 0.05% of xanthan gum, 3% of polyvinyl alcohol and deionized water to complement 100% under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The above formula and process of (1) and (2) are prepared, and xanthan gum is added only as a comparison test.
The suspension performance and the suspension rate of the prepared 30% compound A suspension agent are respectively measured.
Table 730% compound a suspending agent suspension data
Example 8, 25% Etoxazole mite nitrile Compound A suspension
According to the formula requirement, 10% of ethaboxam, 15% of compound A, 49133% of Atlox, 2% of Morwet EFW and 20% of deionized water are respectively treated according to the two process methods (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.15 percent of xanthan gum, 2 percent of polyvinyl alcohol and deionized water are continuously added to complement to 100 percent. The preparation method comprises the steps of firstly carrying out coarse-step dispersing and mixing, then transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 microns to obtain liquid medicine H. (2) Adding the above materials into a mixing tank in sequence for mixing, performing coarse step dispersion mixing, transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering to obtain liquid medicine H when the particle size D50 is less than or equal to 2 micrometers. And (3) dispersing and stirring the liquid medicine H, keeping the rotating speed to be more than 20rpm, adding 0.15% of xanthan gum, 2% of polyvinyl alcohol and 100% of deionized water to complement under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The above formula and process of (1) and (2) are prepared, and xanthan gum is added only as a comparison test.
And respectively measuring the suspension performance and the suspension rate of the prepared 25% ethacrylonitrile-compound A suspending agent.
TABLE 825% Etoxazole mite nitrile, Compound A suspending agent suspension data
Example 9, 30% Etoxazole mite nitrile Compound A suspending agent
According to the formula requirement, 20% of ethacrylonitrile, 10% of compound A, SK-245%, Morwet EFW 2% and 13% of deionized water are respectively treated according to the two process methods (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.05 percent of xanthan gum, 1 percent of polyvinyl alcohol and deionized water are continuously added to complement to 100 percent. The preparation method comprises the steps of firstly carrying out coarse-step dispersing and mixing, then transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 microns to obtain the liquid medicine I. (2) Adding the above materials into a mixing tank in sequence for mixing, performing coarse step dispersion mixing, transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering to obtain the liquid medicine I when the particle size D50 is less than or equal to 2 micrometers. And (3) dispersing and stirring the liquid medicine I, keeping the rotating speed to be more than 20rpm, adding 0.05% of xanthan gum, 1% of polyvinyl alcohol and deionized water to complement 100% under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The above formula and process of (1) and (2) are prepared, and xanthan gum is added only as a comparison test.
And respectively measuring the suspension performance and the suspension rate of the prepared 30% ethaconazole-acaricidal nitrile-compound A suspending agent.
Table 930% ethacrylonitrile, compound a suspension data
Example 10, 35% Etoxazole mite nitrile Compound A suspending agent
According to the formula requirement, 30% of ethaboxam, 5% of compound A, 4% of NNO, 2% of Morwet EFW and 9% of deionized water are respectively treated according to the two process methods (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.02 percent of xanthan gum, 3 percent of polyvinyl alcohol and deionized water are continuously added to complement to 100 percent. The preparation method comprises the steps of firstly dispersing and mixing in a coarse step, then transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 microns to obtain liquid medicine J. (2) Adding the above-mentioned material in proper order into the blending tank and mixing, earlier through the coarse step dispersion mix, then shift into the sand mill and carry out the sanding, detect the granularity of sanding material with the particle size distribution appearance, after particle diameter D50 is less than or equal to 2 microns, filter, obtain liquid medicine J. And (3) dispersing and stirring the liquid medicine J, keeping the rotating speed to be more than 20rpm, adding 0.02% of xanthan gum, 3% of polyvinyl alcohol and the balance of deionized water to 100% under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The above formula and process of (1) and (2) are prepared, and xanthan gum is added only as a comparison test.
And respectively measuring the suspension performance and the suspension rate of the prepared 35% ethacrylonitrile-compound A suspending agent.
Table 1035% ethiprole compound a suspending agent suspension data
Example 11, 40% Etoxazole mite nitrile Compound A suspension
According to the formula requirement, 20% of ethaboxam, 20% of compound A, 5% of Atlox, 1% of Morwet EFW and 4% of deionized water are respectively treated according to the two process methods (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.01 percent of xanthan gum, 4 percent of polyvinyl alcohol and deionized water are continuously added to complement to 100 percent. The preparation method comprises the steps of firstly dispersing and mixing in a coarse step, then transferring into a sand mill for sanding, detecting the granularity of the sanded material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 microns to obtain the liquid medicine K. (2) Adding the above-mentioned material into blending tank in proper order and mixing, firstly through the coarse step dispersion mixing, then transferring into the sand mill and carrying out the sanding, detect the granularity of sanding material with the particle size distribution appearance, after particle diameter D50 is less than or equal to 2 microns, filter, obtain liquid medicine K. And (3) dispersing and stirring the liquid medicine K, keeping the rotating speed to be more than 20rpm, adding 0.01% of xanthan gum, 4% of polyvinyl alcohol and deionized water to complement 100% under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The above formula and process of (1) and (2) are prepared, and xanthan gum is added only as a comparison test.
And respectively measuring the suspension performance and the suspension rate of the prepared 40% ethacrilonitrile-compound A suspension agent.
TABLE 1140% Chlorobipyr, Compound A suspending agent suspension data
Example 12, 45% Etoxazole mite nitrile Compound A suspension
According to the formula, 30% of the flufenpyr-diethyl, 15% of the compound A, GY-D072%, SP 27282% and 11% of deionized water are respectively treated according to the two process methods of (1) and (2). (1) The materials are sequentially added into a mixing tank to be mixed, 0.02 percent of xanthan gum, 1 percent of polyvinyl alcohol and deionized water are continuously added to complement to 100 percent. Firstly, dispersing and mixing in a coarse step, then transferring into a sand mill for sand milling, detecting the granularity of the sand-milled material by using a granularity distribution instrument, and filtering when the particle size D50 is less than or equal to 2 micrometers to obtain the liquid medicine L. (2) The preparation method comprises the steps of sequentially adding the substances into a mixing tank for mixing, dispersing and mixing through a coarse step, then transferring into a sand mill for sand milling, detecting the granularity of a sand-milled material by using a granularity distribution instrument, and filtering after the particle size D50 is less than or equal to 2 micrometers to obtain liquid medicine L. And (3) dispersing and stirring the liquid medicine L, keeping the rotating speed to be more than 20rpm, adding 0.02% of xanthan gum, 1% of polyvinyl alcohol and deionized water to complement 100% under the stirring condition, and dispersing and mixing until the xanthan gum and the polyvinyl alcohol are completely dissolved.
The above formula and process of (1) and (2) are prepared, and xanthan gum is added only as a comparison test.
The suspension performance and the suspension rate of the prepared 45% of compound A suspension agent are respectively measured.
TABLE 1245% Compound A suspending agent suspension data
In order to verify the efficacy of the acaricide suspension prepared, the following biological activity tests were carried out in which the biological activity against Tetranychus cinnabarinus of example 1(A-1/A-2/A-3/A-4/A-5) and example 5(E-1/E-2/E-3/E-4/E-5) were compared.
Example 13 Tetranychus cinnabarinus bioactivity test-1
Reagent to be tested: a-1, A-2, A-3 and A-4 in example 1.
The test conditions are as follows: insecticide laboratory, normal room temperature. The temperature, humidity and illumination of the pesticide observation chamber can be adjusted as required. Greenhouse, all-weather sunlight greenhouse.
Preparing a liquid medicine: the tested medicament is accurately weighed by an electronic analytical balance, the preparation is directly added with water to prepare mother liquor with required concentration, and the mother liquor is respectively diluted into a series of liquid medicines with certain concentration gradient by water according to the experimental design.
The test method comprises the following steps: the activity of different batches of test samples on tetranychus cinnabarinus adults is determined by a potted seedling spraying method. Firstly, inoculating tetranychus cinnabarinus with consistent size to kidney bean seedling leaves in a first true leaf flattening period, and counting the base number after the tetranychus cinnabarinus is stabilized; then, the mixture is evenly sprayed according to the sequence from low dose to high dose according to the experimental design, each plant is 2mL, and a blank control is additionally arranged.
The investigation method comprises the following steps: placing the treated test material in an observation room with certain conditions, periodically investigating the number of dead and alive mites, calculating the mortality, and calculating a toxicity regression equation and LC (liquid chromatography) by using DPS (data processing System) software50Values and 95% confidence limits.
TABLE 13 indoor toxicity determination of Tetranychus cinnabarinus for tetranychus cinnabarinus
As can be seen from Table 13, the agent samples under different suspension performance conditions have obvious difference on the indoor toxicity results of Tetranychus cinnabarinus, wherein A-5 is the conventional preparation method of the conventional suspending agent, no suspending substance is added, the LC50 value is the largest, and the toxicity is low and the pharmacodynamic activity is the worst. A-3 and A-4 are prepared by adding different suspending substances at specific time points by the method (II), and the acaricidal activity is obviously better than that of A-5 and the activities of A-1 and A-2 prepared by the conventional method (I); meanwhile, the control effect of the xanthan gum-polyvinyl alcohol-added combination A-3 and the individual xanthan gum A-4 is better and outstanding.
Example 14 Tetranychus cinnabarinus bioactivity test-2
Reagent to be tested: example 5 includes E-1, E-2, E-3, E-4 and E-5.
The test conditions are as follows: insecticide laboratory, normal room temperature. The temperature, humidity and illumination of the pesticide observation chamber can be adjusted as required. Greenhouse, all-weather sunlight greenhouse.
Preparing a liquid medicine: the tested medicament is accurately weighed by an electronic analytical balance, the preparation is directly added with water to prepare mother liquor with required concentration, and the mother liquor is respectively diluted into a series of liquid medicines with certain concentration gradient by water according to the experimental design.
The test method comprises the following steps: the activity of different batches of test samples on tetranychus cinnabarinus adults is determined by a potted seedling spraying method. Firstly, inoculating tetranychus cinnabarinus with consistent size to kidney bean seedling leaves in a first true leaf flattening period, and counting the base number after the tetranychus cinnabarinus is stabilized; then, the mixture is evenly sprayed according to the sequence from low dose to high dose according to the experimental design, each plant is 2mL, and a blank control is additionally arranged.
The investigation method comprises the following steps: placing the treated test material in an observation room under certain conditions, periodically investigating the number of dead and live mites, calculating the mortality, and calculating a toxicity regression equation and LC (inductance capacitance) by using DPS (data processing system) software50Values and 95% confidence limits.
TABLE 14 indoor toxicity assay for tetranychus cinnabarinus to tetranychus cinnabarinus
As can be seen from Table 14, the agent samples under different suspension performance conditions have obvious difference on the indoor toxicity results of Tetranychus cinnabarinus, wherein E-5 is the conventional preparation method of the conventional suspending agent, no suspending substance is added, the LC50 value is the largest, and the low toxicity and the worst pharmacodynamic activity are indicated. E-3 and E-4 are different suspending substances added at specific time points by adopting the method (II), and the acaricidal activity is obviously better than that of E-5 and the activities of E-1 and E-2 prepared by the conventional method (I); meanwhile, the control effect of the xanthan gum-polyvinyl alcohol-added combination A-3 and the individual xanthan gum A-4 is better and outstanding.
By combining the above examples, it can be seen that the suspension performance and the suspension rate of the suspension system formulation are indeed obviously related to the drug effect, and the suspension performance and the suspension rate are improved in the development process of the suspension agent formulation, so that the drug effect is obviously improved. The suspension preparation obtained by the technical means of the invention has better suspension performance and suspension rate.
The acaricides described in the above embodiments are merely representative, and the content of the present invention can be applied to improvement of suspension performance and suspension rate of other acaricides. Those not described in detail in this specification are within the skill of the art.
Claims (5)
1. An acaricide suspending agent, effective active ingredients and an auxiliary agent, wherein the effective active ingredients are compounds with acaricidal activity, and the acaricide suspending agent is characterized in that: the suspending agent contains suspending agent in the amount of 0.01-10 wt%, which is xanthan gum and/or polyvinyl alcohol.
2. An acaricide suspension concentrate as described in claim 1, wherein: the addition amount of the xanthan gum accounts for 0.01-0.3% of the weight of the preparation; the addition amount of the polyvinyl alcohol accounts for 1 to 5 percent of the weight of the preparation.
3. An acaricide suspension concentrate as described in claim 1 or 2, characterized in that: the effective active ingredients are selected from one or more of chlormequat, spirotetramat and a compound A; wherein, the structural formula of the compound A is as follows
4. An acaricide suspension concentrate according to claim 3, characterized in that: the effective active ingredients of the suspending agent account for 5-60% of the weight of the preparation.
5. A method for producing an acaricide suspension according to claim 1, characterized in that: mixing other components except suspending agent proportionally, dispersing uniformly, sanding until particle diameter D50 is less than 2 μm to obtain liquid medicine stock solution, adding suspending agent xanthan gum into the liquid medicine stock solution proportionally in a mixing and stirring manner, mixing uniformly, adding polyvinyl alcohol, and dispersing uniformly to obtain acaricide suspending agent.
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