CN114258916B - JuncJing compound boscalid suspending agent and preparation method and application thereof - Google Patents
JuncJing compound boscalid suspending agent and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of pesticide preparations, and in particular relates to a dimethachlon compound boscalid suspending agent, a preparation method and application thereof, wherein the suspending agent comprises dimethachlon 5-40% by weight; 5-30% of boscalid; 1-20% of wetting dispersant; 0.1-2% of defoaming agent; 0.1-5% of thickener; 1-10% of an antifreezing agent; 0.01-5% of stabilizer; 0-10% of penetration enhancer; the deionized water is filled up to 100%; the mass ratio of the dimethachlon to the boscalid is 4:1-1:1.5. The suspension preparation of the invention is characterized in that the dimethachlon and boscalid are reasonably compounded, water is used for replacing solid powdery filler, and each active ingredient of the suspension is uniformly dispersed in water by the physical dispersion action of a dispersing agent and a sand mill to form a white suspension, and the preparation method has the advantages of simple process, low production cost, high efficiency, stability, low toxicity, no pollution, safety and environmental friendliness to people and livestock, suitability for grape gray mold control and good effect.
Description
Technical Field
The invention belongs to the technical field of pesticide preparations, and particularly relates to a dimethachlon compound boscalid suspending agent, a preparation method and application thereof.
Background
The dimethachlon is a protective bactericide and has a certain systemic treatment effect. Is mainly used for preventing and treating rice sheath blight disease, sclerotinia rot of colza and tobacco brown spot, for example, preventing and treating sclerotinia rot of colza 1 times by 4.5-7.5g/100m 2 2 times 6-15g/100m 2 The control effect is 90-100%.
The dimethachlon is a recognized excellent bactericide, and the main formulation of the dimethachlon is mainly wettable powder. Modern pesticide formulations are evolving towards water-based, ultra-micro, dust-free and controlled release, where water-based is one of the main directions of pesticide development. The suspending agent using water as a carrier can reduce the dosage of an organic solvent, has no dust pollution caused by wettable powder and powder, reduces the production cost of pesticides, and becomes an extremely important dosage form in pesticide preparations.
Boscalid is a novel nicotinamide fungicide developed by basf corporation in germany, and is mainly used for controlling powdery mildew, gray mold, various rot diseases, brown rot and root rot, etc., which have been registered in the united kingdom, germany and switzerland in 2004. Boscalid belongs to a succinate coenzyme Q reductase inhibitor in the mitochondrial respiratory chain, has strong inhibition capability on spore germination, and has no cross resistance with other bactericides. Boscalid is a novel nicotinamide fungicide, has a wide sterilization spectrum, is almost active on all types of fungal diseases, is very effective on controlling powdery mildew, gray mold, sclerotium disease, various rot diseases and the like, is also effective on resistant bacteria of other medicaments, is mainly used for controlling diseases including rape, grape, fruit trees, vegetables, field crops and the like, but has higher single use cost. Although the preparation of the dimethachlon and the boscalid has been reported in a related way, how to compound the boscalid to achieve the effect when the boscalid is used alone is worthy of research.
The suspending agent is an environment-friendly green formulation, has the characteristics of safe production, convenient use, high suspension rate and strong adhesive force, is one of main development directions of pesticide preparations, has increasingly large production scale and has higher and higher acceptance of terminal clients.
In the production process of the suspending agent, xanthan gum is generally used as one of the thickening agents, and at present, two modes of adding the xanthan gum are adopted, wherein one mode is that the xanthan gum is mixed into materials and then made into paddles, and the paddles are sanded together to directly obtain the suspending agent; the other is to use water as a dissolving agent to select xanthan gum to be dissolved into 1-2% of aqueous solution, then to add the aqueous solution into sanded materials in proportion to be uniformly mixed to prepare a suspending agent, and the suspending agent prepared by the method is characterized in that the quality of the suspending agent is controllable, but the phenomenon of incomplete dissolution or longer time consumption is easy to occur in the dissolving process due to the special physicochemical property of the xanthan gum, the production period is long, and the phenomenon of unstable quality is easy to occur.
In view of the above, it is necessary to research a dimethachlon compound boscalid suspending agent with good and stable control effect, low cost and simple process.
Disclosure of Invention
The invention aims to provide a dimethachlon compound boscalid suspending agent, a preparation method and application thereof, wherein the dimethachlon compound boscalid suspending agent is prepared by reasonably compounding dimethachlon and boscalid, water is used for replacing solid powdery filler, each active ingredient of the suspending agent is uniformly dispersed in water by means of the physical dispersion action of a dispersing agent and a sand mill to form a white suspending agent, the preparation method is simple in process, low in production cost, and the obtained suspending agent is efficient and stable, low in toxicity, pollution-free, safe and friendly to environment, people and livestock, suitable for grape gray mold control and good in effect.
The invention provides a dimethachlon compound boscalid suspending agent, which comprises the following components in percentage by weight:
the mass ratio of the dimethachlon to the boscalid is 4:1-1:1.5.
Preferably, in the above technical scheme, the mass ratio of the dimethachlon to the boscalid is 2:1-1:1.
Preferably, in the above technical solution, the particle size of the suspending agent is less than 15 μm. According to the technical scheme, the particle size of the suspending agent is controlled to be smaller than 15 mu m, the suspending agent is easier to disperse, no sedimentation layer bottom phenomenon exists, fine particles can be distributed on the surface of crops after spraying when the suspending agent is used, the suspending agent is uniformly dispersed on a target, and the prevention and control effect is good.
Preferably, in the above technical scheme, the wetting dispersant is one or more of sodium laureth sulfate, sodium dodecyl sulfate, potassium oleate, polyoxyethylene polyoxypropylene ether block copolymer, sodium polyethanecarboxylate, dodecyl polyoxyethylene ether phosphate, alkyl naphthalene formaldehyde condensate sulfonate, sodium oleate methyl aminoethyl sulfonate, starch, gelatin, hydroxymethyl cellulose and polyvinyl alcohol.
Preferably, in the above technical scheme, the thickener is a composition of xanthan gum and any one or more of magnesium aluminum silicate, heteropolysaccharide, hydroxymethyl cellulose, methyl cellulose, acacia, sodium alginate, pectin, polyvinyl alcohol and bentonite. In the technical scheme, the composition of the xanthan gum and other thickening agents is used, so that the suspension stability of the preparation can be improved, the quality is controllable, and the xanthan gum accounts for 3-15% of the using amount of the thickening agents preferentially.
Preferably, in the above technical scheme, the stabilizer is one or more of pyrogallol, butyl glycidyl ether, phenyl glycidyl ether, tolyl glycidyl ether, polyvinyl glycol diglycidyl ether, sodium sorbate, sodium benzoate, epoxidized soybean oil, linseed oil, eugenol, ascorbic acid, castor oil, olive oil, hydroquinone, salicylic acid and benzisothiazolinone.
Preferably, in the above technical solution, the penetration enhancer is one or two of laurocapram and fatty alcohol polyoxyethylene ether (JFC); the defoamer is any one of silicone oil, silicone, C10-20 saturated fatty acid and C8-10 fatty alcohol.
Preferably, in the above technical scheme, the antifreezing agent is polyethylene glycol-200.
The invention also provides a preparation method of the dimethachlon compound boscalid suspending agent, which comprises the following steps:
s1, dissolving xanthan gum by taking an antifreezing agent as a solvent, adding a proper amount of deionized water after the xanthan gum is completely dissolved, and rapidly stirring to prepare 1-2% xanthan gum aqueous solution;
s2, placing the dimethachlon and boscalid raw material, a wetting dispersant, a thickening agent except xanthan gum, a stabilizing agent, a defoaming agent, a penetration enhancer and 90-95% of the rest deionized water after water required for preparing the xanthan gum is subtracted in a preparation tank, uniformly mixing to prepare slurry, and then placing the slurry in a sand mill, and performing sand milling until the particle size is smaller than 15 mu m to obtain a sand milling material;
s3, adding the xanthan gum aqueous solution obtained in the step S1 into the sanding material obtained in the step S2 in proportion, cleaning a pipeline and equipment by using the rest 5-10% deionized water, adding flushing liquid into the preparation mixed with the xanthan gum aqueous solution, uniformly mixing, and sampling and detecting to be qualified.
In the technical scheme, the polyethylene glycol-200 antifreeze fluid is used as the solvent of the xanthan gum, so that the solution is completely dissolved and fast, the original chemical chain is reserved without sanding, the stability is good, and meanwhile, the use of the antifreeze fluid can improve the compounding property of the suspending agent; water is used as a solvent, and simultaneously, solid powdery filler is replaced, so that an organic solvent is not used, and the environment is protected; the water is used in batches, meanwhile, water for flushing equipment is reserved, the recovery rate of the medicament is high, and no wastewater is generated; by separate dissolution and final mixing, the stability of the suspending agent can be improved.
The invention also provides application of the suspending agent in preventing and controlling grape gray mold. Specifically, when the dimethachlon and boscalid suspending agent is used for preventing and treating grape gray mold, the medicament with the dosage of 800-1000 times of the preparation is used, and the application mode adopts foliar spraying, generally spraying for 2 times at intervals of 7-10 days. The uniformity of spraying medicine should be noted during application, especially the inflorescence and the ear should be uniformly applied, and the spraying should be performed once during grape fruit color transfer period when diseases seriously occur.
Compared with the prior art, the beneficial effects are that:
1. the suspension preparation of the invention reasonably compounds the dimethachlon and boscalid, replaces solid powdery filler with water, and uniformly disperses each active ingredient of the suspension agent into water by fine particles under the physical dispersion action of a dispersing agent and a sand mill to form a white suspension agent.
2. In the preparation process, each active ingredient of the suspending agent is uniformly dispersed in water with the particle size smaller than 15 mu m, and the suspending agent has the following advantages: (1) the dust is less, the environmental pollution is small, and the production and the use are safe; (2) the flash point is high, the combustion and explosion are avoided, and the production, storage and use are safe; (3) the water is used as a matrix, so that the resource is rich, the product cost is low, and the packaging is easy; (4) the suspending agent prepared by taking polyethylene glycol-200 as an antifreezing agent not only can meet the antifreezing requirement, but also can provide support for rapidly preparing 1-2% xanthan gum aqueous solution, and the suspending agent prepared by taking polyethylene glycol-200 as the antifreezing agent has higher miscibility; (5) the residual water required by the cleaning equipment is reserved in advance, and equipment materials are recycled, so that the yield of finished products of the preparation is improved, the waste water is reduced, and the environmental protection pressure is reduced; (6) after the preparation is used for spraying, the preparation is distributed on the surface of crops in the form of fine particles, so that the preparation is better in dispersion on a target, good in control effect and good in economic benefit.
3. The dimethachlon and boscalid suspending agent prepared by the invention has good control effect on grape gray mold, the control effect reaches more than 90 percent, the dimethachlon and boscalid suspending agent is obviously superior to the single 40 percent dimethachlon wettable powder, has equivalent control effect to 50 percent boscalid water dispersible granule, can reduce the use amount of boscalid and has low cost.
Drawings
FIG. 1 is a process flow diagram of a method of preparing a suspending agent according to the present invention.
Detailed Description
The above-described features of the invention and those specifically described in the following (example embodiments) may be combined with each other to constitute new or preferred embodiments, but the invention is not limited to these embodiments, nor is they limited to them in any way.
The experimental methods in the following examples are conventional methods unless otherwise specified. The preparations according to the examples below are commercially available and are commercially available unless otherwise specified.
The invention is described in further detail below with reference to examples:
example 1:28% dimethachlon+14% boscalid suspending agent
The dimethachlon compound boscalid suspending agent comprises the following components in percentage by weight:
the preparation method comprises the following steps:
s1, dissolving xanthan gum by taking an antifreezing agent as a solvent, adding a proper amount of deionized water after the xanthan gum is completely dissolved, and rapidly stirring to prepare 1-2% xanthan gum aqueous solution;
s2, placing the dimethachlon and boscalid raw material, a wetting dispersant, a thickener except xanthan gum, a stabilizer, a defoaming agent, a penetration enhancer and 90% of the rest deionized water which is used for preparing the xanthan gum after water is subtracted in a preparation tank, uniformly mixing to prepare slurry, and then placing the slurry in a sand mill, and grinding until the particle size is all smaller than 15 mu m to obtain a grinding material;
s3, adding the xanthan gum aqueous solution obtained in the step S1 into the sanding material obtained in the step S2 in proportion, cleaning a pipeline and equipment by using the rest 10% deionized water, adding flushing liquid into a preparation mixed with the xanthan gum aqueous solution, and uniformly mixing to obtain the 28% dimethachlon+14% boscalid suspending agent.
Example 2:30% dimethachlon+10% boscalid suspending agent
The dimethachlon compound boscalid suspending agent comprises the following components in percentage by weight:
the preparation method comprises the following steps:
s1, dissolving xanthan gum by taking an antifreezing agent as a solvent, adding a proper amount of deionized water after the xanthan gum is completely dissolved, and rapidly stirring to prepare 1-2% xanthan gum aqueous solution;
s2, placing the dimethachlon and boscalid raw material, a wetting dispersant, a thickener except xanthan gum, a stabilizer, a defoaming agent, a penetration enhancer and 90% of the rest deionized water which is used for preparing the xanthan gum after water is subtracted in a preparation tank, uniformly mixing to prepare slurry, and then placing the slurry in a sand mill, and grinding until the particle size is all smaller than 15 mu m to obtain a grinding material;
s3, adding the xanthan gum aqueous solution obtained in the step S1 into the sanding material obtained in the step S2 in proportion, cleaning a pipeline and equipment by using the rest 10% deionized water, adding flushing liquid into a preparation mixed with the xanthan gum aqueous solution, and uniformly mixing to obtain the 30% dimethachlon+10% boscalid suspending agent.
Example 3:40% dimethachlon+10% boscalid suspending agent
The dimethachlon compound boscalid suspending agent comprises the following components in percentage by weight:
the preparation method comprises the following steps:
s1, dissolving xanthan gum by taking an antifreezing agent as a solvent, adding a proper amount of deionized water after the xanthan gum is completely dissolved, and rapidly stirring to prepare 1-2% xanthan gum aqueous solution;
s2, placing the dimethachlon and boscalid raw material, a wetting dispersant, a thickener except xanthan gum, a stabilizer, a defoaming agent, a penetration enhancer and 95% of residual deionized water which is used for preparing the xanthan gum and is removed from water required for preparing the xanthan gum into a preparation tank, uniformly mixing to prepare slurry, and then placing the slurry into a sand mill, and grinding until the particle size is all smaller than 15 mu m to obtain a sand-ground material;
s3, adding the xanthan gum aqueous solution obtained in the step S1 into the sanding material obtained in the step S2 in proportion, cleaning a pipeline and equipment by using the rest 5% deionized water, adding flushing liquid into a preparation mixed with the xanthan gum aqueous solution, and uniformly mixing to obtain the 40% dimethachlon+10% boscalid suspending agent.
Example 4:20% dimethachlon+30% boscalid suspending agent
The dimethachlon compound boscalid suspending agent comprises the following components in percentage by weight:
the preparation method comprises the following steps:
s1, dissolving xanthan gum by taking an antifreezing agent as a solvent, adding a proper amount of deionized water after the xanthan gum is completely dissolved, and rapidly stirring to prepare 1-2% xanthan gum aqueous solution;
s2, placing the dimethachlon and boscalid raw material, a wetting dispersant, a thickener except xanthan gum, a stabilizer, a defoaming agent, a penetration enhancer and 95% of residual deionized water which is used for preparing the xanthan gum and is removed from water required for preparing the xanthan gum into a preparation tank, uniformly mixing to prepare slurry, and then placing the slurry into a sand mill, and grinding until the particle size is all smaller than 15 mu m to obtain a sand-ground material;
s3, adding the xanthan gum aqueous solution obtained in the step S1 into the sanding material obtained in the step S2 in proportion, cleaning a pipeline and equipment by using the rest 5% deionized water, adding flushing liquid into a preparation mixed with the xanthan gum aqueous solution, and uniformly mixing to obtain the 20% sclerotin+30% boscalid suspending agent.
Comparative example 1:28% dimethachlon+14% boscalid suspending agent
The dimethachlon compound boscalid suspending agent comprises the following components in proportion as in example 1.
The preparation method comprises the following steps:
s1, dissolving xanthan gum by taking water as a solvent, and preparing 1-2% xanthan gum aqueous solution after the xanthan gum is completely dissolved by rapid stirring;
s2, placing the dimethachlon and boscalid raw material, a wetting dispersant, a thickener except xanthan gum, a stabilizer, a defoaming agent, a penetration enhancer, an antifreezing agent and 90% of the rest deionized water after water required for preparing the xanthan gum is subtracted in a preparation tank, uniformly mixing to prepare slurry, and then placing the slurry in a sand mill, and grinding until the particle size is smaller than 15 mu m to obtain a sand grinding material;
s3, adding the xanthan gum aqueous solution obtained in the step S1 into the sanding material obtained in the step S2 in proportion, cleaning a pipeline and equipment by using the rest 10% deionized water, adding flushing liquid into a preparation mixed with the xanthan gum aqueous solution, and uniformly mixing to obtain the 28% dimethachlon+14% boscalid suspending agent.
Comparative example 2:28% dimethachlon+14% boscalid suspending agent
The dimethachlon compound boscalid suspending agent comprises the following components in proportion as in example 1.
The preparation method comprises the following steps:
s1, placing the dimethachlon and boscalid raw material, a wetting dispersant, a thickener except xanthan gum, a stabilizer, a defoamer, xanthan gum, a penetration enhancer, an antifreezing agent and 90% deionized water into a preparation tank, uniformly mixing to prepare slurry, and then placing the slurry into a sand mill, and grinding until the particle size is all smaller than 15 mu m to obtain a sand-ground material;
s2, cleaning a pipeline and equipment by using the rest 10% deionized water, adding flushing liquid into the sand grinding material obtained in the step S1, and uniformly mixing to obtain the 28% sclerotinia+14% boscalid suspending agent.
Comparative example 3:28% dimethachlon+14% boscalid suspending agent
The dimethachlon compound boscalid suspending agent comprises the following components in proportion as in example 1.
The preparation method comprises the following steps:
s1, dissolving xanthan gum by taking an antifreezing agent as a solvent, adding a proper amount of deionized water after the xanthan gum is completely dissolved, and rapidly stirring to prepare 1-2% xanthan gum aqueous solution;
s2, uniformly mixing the dimethachlon and boscalid raw materials with a wetting dispersant, a thickener except xanthan gum, a stabilizer, a defoaming agent, a penetration enhancer and 90% of residual deionized water after water required for preparing the xanthan gum is subtracted in a preparation tank to prepare slurry, and then placing the slurry in a sand mill, and grinding until the particle size is larger than 20 mu m to obtain a grinding material;
s3, adding the xanthan gum aqueous solution obtained in the step S1 into the sanding material obtained in the step S2 in proportion, cleaning a pipeline and equipment by using the rest 10% deionized water, adding flushing liquid into a preparation mixed with the xanthan gum aqueous solution, and uniformly mixing to obtain the 28% sclerotin+14% boscalid suspending agent
The suspending agents obtained in examples 1 to 4 and comparative examples 1 to 3 were tested for their suspension rate according to the GB/T14825-2006 method for measuring the suspension rate of pesticides, and the results are shown in Table 1.
TABLE 1 suspension Rate
| Group of | Suspension percentage (%) | Others |
| Example 1 | 98.6 | Has good stability and no layering phenomenon |
| Example 2 | 98.3 | Has good stability and no layering phenomenon |
| Example 3 | 97.8 | Has good stability and no layering phenomenon |
| Example 4 | 98.4 | Has good stability and no layering phenomenon |
| Comparative example 1 | 89.8 | Has good stability and no obvious layering phenomenon |
| Comparative example 2 | 73.3 | Poor stability, layering and bottoming |
| Comparative example 3 | 79.5 | Poor stability, layering and bottoming |
As can be seen from the results in Table 1, the suspending agent prepared by the method of the invention has high suspension property and stability and good product quality. As can be seen from the results of examples 1 and comparative examples 1 to 3, the suspension property of the obtained product can be obtained by dissolving xanthan gum in water in advance, but the water solubility of xanthan gum is poor, the dissolving process is longer, and the effect of the suspending agent obtained in example 1 is slightly poorer; directly mixing xanthan gum with other components and then sanding to obtain a suspending agent with poor stability and easy layering; when the particle diameter of the suspending agent exceeds 15. Mu.m, suspension is not facilitated and stability is poor.
Test example 1: combined virulence assay
Test target: grape gray mold (Botrytis cinerea)
The test method comprises the following steps: indoor virulence was determined using the growth rate method. According to the solubility of the dimethachlon and boscalid in the solvent, acetone is selected for dissolution, and after dissolution, the dimethachlon and boscalid are diluted by 0.1% Tween 80 aqueous solution. And (3) preparing single-dose mother solutions respectively, designing more than 5 groups of proportions according to the purpose of mixing, mixing before adding a culture medium, and setting 5 series of mass concentrations for the single-dose mixed solution and each group of mixed solution. Specific concentration designs are shown in table 2:
TABLE 2 Junjing+boscalid compounding and pyridine theory design
| Sequence number | Medicament | Proportioning of | Concentration mg/L |
| A | Sclerotium remover | - | 0.5、1.0、2.0、5.0、10.0 |
| B | Boscalid | - | 0.1、0.5、1.0、2.0、5.0、10.0、50.0 |
| 1 | Sclerostin+boscalid | 4:1 | 0.5、1.0、2.0、5.0、10.0 |
| 2 | Sclerostin+boscalid | 3:1 | 0.5、1.0、2.0、5.0、10.0 |
| 3 | Sclerostin+boscalid | 2:1 | 0.5、1.0、2.0、5.0、10.0 |
| 4 | Sclerostin+boscalid | 1.5:1 | 0.5、1.0、2.0、5.0、10.0 |
| 5 | Sclerostin+boscalid | 1:1 | 0.5、1.0、2.0、5.0、10.0 |
| 6 | Sclerostin+boscalid | 1:1.5 | 0.5、1.0、2.0、5.0、10.0 |
The mycelium growth rate method is adopted, the gray mold strain is activated on a sterile PDA culture medium plate, then a puncher is used for beating 5mm fungus dishes on the edge of bacterial colony mycelium growth vigorous, the fungus dishes are moved into the centers of the PDA plate containing the medicament and a blank plate, one fungus cake is arranged on each dish, and each concentration is repeated for 3 times. All plates connected with the bacterial cake are placed in a biochemical incubator and cultivated at a constant temperature of 25 ℃.
The test statistical method comprises the following steps: after the dish is connected, when the blank control is about to grow up to the culture dish, the colony diameter is measured by a crisscross method. Calculating hypha growth inhibition rate, performing regression analysis on concentration logarithmic value and corresponding numerical value of inhibition rate of single dose and mixed agents with different proportions in test by using DPS statistical software, and calculating EC 50 Values and confidence limits.
Calculating the synergistic coefficient (SR) of the mixture according to the Wadley method, wherein the synergistic coefficient SR is more than or equal to 1.5, the compound shows synergy, the synergistic coefficient SR is less than or equal to 0.5, antagonism is shown, and the addition effect is shown as 0.5< SR < 1.5.
Wherein, the mycelium inhibition rate of each pyridine is calculated according to the formula (1), the unit is percentage (%), the calculation result keeps two positions after decimal point, and the theoretical EC of the combined action of the two is calculated 50 Is calculated according to formula (2); the synergy ratio is carried out according to a formula (3).
R＝[(D 0 -D 1 )×100]/(D 0 -N) … … … … (1), wherein: r-hypha growth inhibition (%); d (D) 0 -blank colony diameter; d (D) 1 Colony diameter on plates ordered with the agent; n is the diameter of the fungus disc;
X 1 ＝[(P A +P B )×100]/(P A /A+P B /B) … … … … (2), wherein: x is X 1 EC of the mixture 50 Theoretical values in milligrams per liter (mg/L); p (P) A The percentage of A in the mixture is expressed in percent (%); p (P) B The percentage content of B in the mixture is expressed in percent (%); EC of A in A-mixture 50 Milligrams per liter (mg/L); EC of B in B-mixture 50 Milligrams per liter (mg/L);
SR＝X 1 /X 2 … … … … (3), wherein the SR-synergistic coefficient of the admixture; x is X 1 Mixed agent EC 50 In milligrams per liter (mg/L); x is X 2 Mixed agent EC 50 In milligrams per liter (mg/L).
Test results: the toxicity of dimethachlon, boscalid and their combination on grape gray mold is shown in Table 3.
TABLE 3 toxicity determination results of dimethachlon, boscalid and their combined action on grape gray mold
As can be seen from the test results in Table 3, the SR values of the combined action of 6 mixed agents with different proportions of dimethachlon and boscalid on grape gray mold are both greater than 1 and are 1.1055-1.6205, so that the combined action of the dimethachlon and boscalid is not antagonistic in the range of the test proportion, and the dimethachlon and boscalid belongs to the addition effect or the synergistic effect. Therefore, the two medicaments are mixed to prevent and treat grape gray mold.
In the mixture of the proportions, for the combined action of grape gray mold pathogenic bacteria, when the dimethachlon and boscalid are mixed according to the ratio of 2:1-1:1, the SR value is more than 1.5, and when the SR value is 1.5:1.0 and the SR value is 2.0:1.0, the SR is maximum, and the synergy is most obvious. Therefore, when the two are combined for use in the treatment of botrytis cinerea, it is preferable that the mass ratio of dimethachlon to boscalid is 2:1-1:1.
Test example 2: field district pharmacodynamic test
Test agent: the suspending agent prepared in example 1 is used as a test agent
Test object: grape gray mold (Botrytis cinerea)
Test crop: grape (variety: huge peak)
Test time and place: in 2019, 6 to 9 months, in the sunk-yang Sujia-zon area plastic greenhouse of Shenyang, liaoning province, grape gray mold and downy mildew are common diseases of local grape cultivation in the area with the history of grape planting for many years. The field management is carried out according to the local habit.
And (3) test design: the test design of the test agents is shown in Table 4, cell arrangement: the test agent, the control agent and the blank control are arranged in random groups, 10 plants in each cell with the area of 50 square meters (10 m multiplied by 5 m) are repeated for 4 times.
TABLE 4 test design of reagents for test
The administration mode is as follows: the medicine is applied by a spraying method, and is sprayed by a knapsack sprayer after being uniformly mixed with water, and the medicine is applied twice in the same period, namely, 6 months 12 days and 21 days in 2019 respectively.
Experimental investigation: drug efficacy surveys were conducted 9 days after the first drug administration and 10 days after the last drug administration. At the time of investigation, 10 plants were investigated per cell, 5 inflorescences or clusters were investigated per plant, and the disease portion was classified as a percentage of the entire inflorescence (cluster) area. The grading criteria are as follows in table 5:
TABLE 5 grading Standard
| Level 0 | No disease; |
| level 1 | The diseased part accounts for less than 5% of the whole inflorescence (cluster); |
| 3 grade | The disease part accounts for 6-15% of the whole inflorescence (fruit cluster); |
| grade 5 | The disease part accounts for 16-25% of the whole inflorescence (fruit cluster); |
| level 7 | The disease part accounts for 26-50% of the whole inflorescence (clusters); |
| grade 9 | The diseased part accounts for more than 50 of the whole inflorescence (clusters). |
Statistical analysis method of test data: and counting the data by using Excel and DPS software, analyzing the test data by using a Duncan new complex polar error method (DMRT), and evaluating the test result.
The drug effect calculation method comprises the following steps:
disease index = [ Σ (number of inflorescences (ears) at each stage×number of relative stages) ×100]/[ investigation of total inflorescences (ears) number×number of highest stages ]
Control effect (%) = (control disease index-pyridine disorder disease index) ×100/control disease index
Test results:
(1) The control effect of the field test result (9 days after the first medicine) for controlling grape gray mold is shown in table 6; statistical results of the field trials for controlling grape gray mold (9 days after the first dose) are shown in table 7.
TABLE 6 field test results for controlling grape gray mold (9 days after the first dose)
TABLE 7 statistical results of field trials for controlling grape gray mold (9 days after the first dose)
From the test results in tables 6 and 7, it can be seen that the 42% dimethachlon+boscalid suspending agent has a good control effect on grape gray mold. Investigation is carried out 9 days after the 1 st application, and the control effects of 42% dimethachlon and boscalid suspending agent on grape gray mold are 80.61%, 86.49% and 90.57% respectively under the dilution multiples of 1200, 1000 and 800.
Under the condition that the preparation is diluted by 800 times of boscalid dosage, the control effect of 42% dimethachlon and boscalid suspending agent on grape gray mold is better than that of 40% dimethachlon wettable powder (75.92%) serving as a control medicament, and the effect of the boscalid suspending agent is equivalent to that of 50% boscalid water dispersible granules (92.27%). The effect of the 42% dimethachlon and boscalid suspending agent preparation diluted 1000 times and 1200 times on preventing grape gray mold is better than the effect of the 40% dimethachlon wettable powder diluted 1000 times. The control effect of the 42% dimethachlon and boscalid suspending agent preparation on grape gray mold is obviously different between 1200, 1000 and 800 times of boscalid suspending agent preparation dilution.
(2) The control effect of the field test result (10 days after the second medicine) for controlling grape gray mold is shown in table 8; the statistical results of the field trials for controlling grape gray mold (10 days after the second dose) are shown in table 9.
Table 8 results of field trials for controlling Botrytis cinerea (10 days after the second dose)
Table 9 statistical results of field trials for controlling Botrytis cinerea (10 days after the second dose)
From the data in tables 8 and 9, it can be seen that the test area blank was investigated at 10 days after the 2 nd administration, and the disease state of 42% of the dimethachlon+boscalid suspending agent pyridine management area was controlled. The control effect on grape gray mold is 71.21%, 82.35% and 87.76% respectively under the dilution multiples of 1200, 1000 and 800. Under the condition that the preparation is diluted by 800 times of boscalid dosage, the control effect of 42% dimethachlon and boscalid suspending agent on grape gray mold is better than that of 40% dimethachlon wettable powder (67.33%) serving as a control medicament, and the effect of the boscalid suspending agent is equivalent to that of 50% boscalid water dispersible granules (89.15%). The effect of the 42% dimethachlon and boscalid suspending agent preparation diluted 1000 times and 1200 times on preventing grape gray mold is better than the effect of the 40% dimethachlon wettable powder diluted 1000 times. The control effect of the 42% dimethachlon and boscalid suspending agent preparation on grape gray mold is obviously different between 1200, 1000 and 800 times of boscalid suspending agent preparation dilution.
(3) In the test, the 42% dimethachlon+boscalid suspending agent has no adverse effect on grape growth and environmental organisms at the dilution of the preparation of 800-1200.
In conclusion, the invention combines the dimethachlon and boscalid to prevent and treat the grape gray mold, and the mass ratio is controlled to be 2:1-1:1, so that the invention has a synergistic effect; the suspending agent prepared by the method has high suspension property and stability and good product quality; the 42% dimethachlon+boscalid (2:1) suspending agent has excellent control effect on grape gray mold, and the control effect of the 42% dimethachlon+boscalid suspending agent on grape gray mold is better than that of 40% dimethachlon wettable powder serving as a control agent under the dose of boscalid diluted 800, 1000 and 1200 times; the control effect of the boscalid dose diluted by 800 times on grape gray mold is equivalent to that of 50% boscalid water dispersible granules. Therefore, when 42% dimethachlon+boscalid suspending agent is used for preventing and treating grape gray mold, the dosage of the agent is 800-1000 times of the dosage of the agent, and the application mode is foliar spray, and the spraying is carried out for 2 times at intervals of 7-10 days.
Finally, it should be emphasized that the foregoing description is merely illustrative of the preferred embodiments of the invention, and that various changes and modifications can be made by those skilled in the art without departing from the spirit and principles of the invention, and any such modifications, equivalents, improvements, etc. are intended to be included within the scope of the invention.
Claims (6)
1. The dimethachlon compound boscalid suspending agent is characterized by comprising the following components in percentage by weight:
5-40% of dimethachlon;
5-30% of boscalid;
1-20% of wetting dispersant;
0.1-2% of defoaming agent;
0.1-5% of thickener;
1-10% of an antifreezing agent;
0.01-5% of stabilizer;
0-10% of penetration enhancer;
the deionized water is filled up to 100%;
the mass ratio of the dimethachlon to the boscalid is 2:1;
the thickener is one or more of xanthan gum, magnesium aluminum silicate, heteropolysaccharide, hydroxymethyl cellulose, methyl cellulose, acacia, sodium alginate, pectin, polyvinyl alcohol and bentonite;
the antifreezing agent is polyethylene glycol-200;
the preparation method of the suspending agent comprises the following steps:
s1, dissolving xanthan gum by taking an antifreezing agent as a solvent, adding a proper amount of deionized water after the xanthan gum is completely dissolved, and rapidly stirring to prepare 1-2% xanthan gum aqueous solution;
s2, placing the dimethachlon and boscalid raw material, a wetting dispersant, a thickening agent except xanthan gum, a stabilizing agent, a defoaming agent, a penetration enhancer and 90-95% of the rest deionized water after water required for preparing the xanthan gum is subtracted in a preparation tank, uniformly mixing to prepare slurry, and then placing the slurry in a sand mill, and performing sand milling until the particle size is smaller than 15 mu m to obtain a sand milling material;
s3, adding the xanthan gum aqueous solution obtained in the step S1 into the sanding material obtained in the step S2 in proportion, cleaning a pipeline and equipment by using the rest 5-10% deionized water, adding flushing liquid into the preparation mixed with the xanthan gum aqueous solution, uniformly mixing, and sampling and detecting to be qualified.
2. The dimethachlon compound boscalid suspension of claim 1, wherein the particle size of the suspension is less than 15 μm.
3. The dimethachlon compound boscalid suspending agent according to claim 1, wherein the wetting dispersant is one or more of sodium laureth sulfate, sodium dodecyl sulfate, potassium oleate, polyoxyethylene polyoxypropylene ether block copolymer, sodium polyethanecarboxylate, dodecyl polyoxyethylene ether phosphate, alkyl naphthalene formaldehyde condensate sulfonate, sodium methyl amino ethyl oleate sulfonate, starch, gelatin, hydroxymethyl cellulose and polyvinyl alcohol.
4. The dimethachlon compound boscalid suspending agent according to claim 1, wherein the stabilizer is one or more of pyrogallol, butyl glycidyl ether, phenyl glycidyl ether, tolyl glycidyl ether, polyethylene glycol diglycidyl ether, sodium sorbate, sodium benzoate, epoxidized soybean oil, linseed oil, eugenol, ascorbic acid, castor oil, olive oil, hydroquinone, salicylic acid and benzisothiazolinone.
5. The dimethachlon compound boscalid suspending agent according to claim 1, wherein the penetration enhancer is one or two of laurocapram and fatty alcohol-polyoxyethylene ether; the defoamer is organic silicone oil, silicone and C 10-20 Saturated fatty acids, C 8-10 Any one of fatty alcohols.
6. Use of the suspension according to any one of claims 1 to 5 for controlling grape gray mold.
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