A water-dispersible granule containing diclofenac and its preparation method

Abstract

This invention relates to the field of pesticide technology and proposes a water-dispersible granule containing bispyribac-methyl and its preparation method, comprising the following raw materials in parts by weight: 50-60 parts of active ingredient, 6-8 parts of dispersant, 5-10 parts of disintegrant, 2-4 parts of wetting agent, 1-2 parts of defoamer, 2-4 parts of binder, and 10-12 parts of filler; the active ingredient is composed of bispyribac-methyl and isoxazoline, and the dispersant includes 2-cyclohexylaminoethanesulfonic acid and / or sulfonate. This technical solution solves the problems of poor dispersibility and slow disintegration rate of water-dispersible granules in related technologies.

Description

Technical Field

[0001] This invention relates to the field of pesticide technology, specifically to a water-dispersible granule containing bispyribac-methyl and its preparation method. Background Technology

[0002] Aphids and whiteflies are common agricultural pests. They suck the sap from plants with their piercing-sucking mouthparts, causing leaves to lose their green color, curl, grow slowly, and even die. They not only directly affect plant growth, but also spread viral diseases, further aggravating the damage to plants.

[0003] Bifenthrin is a highly effective insecticide that primarily controls pests through contact and stomach poison action. This drug is very effective against many piercing-sucking pests. Its mechanism of action includes interfering with the insect's chordate organ function, causing the insect to lose its sensitivity to gravity, balance, sound, position, and movement. This results in deafness, loss of coordination and orientation, ultimately preventing the insect from feeding and leading to dehydration and starvation.

[0004] Isoxazolidinamide belongs to the diaryl isoxazoline class of compounds and has good control effects on a variety of pests and mites. Its mechanism of action is relatively unique, involving specific receptors in the insect nervous system. It mainly disrupts the normal transmission of nerve impulses in pests, causing excessive excitement and convulsions, ultimately leading to the death of the pests.

[0005] There are few reports on insecticides containing bispyribac-methyl and isoxaflutole, and currently, insecticide dispersible granules have problems with poor dispersibility and slow disintegration rate, which not only affects the effectiveness of the active ingredients, but also increases the amount of insecticide applied in order to achieve the expected insecticidal effect, causing environmental pollution. Summary of the Invention

[0006] This invention proposes a water-dispersible granule containing bispyribac-methyl and its preparation method, which solves the problems of poor dispersion performance and slow disintegration rate of water-dispersible granules in related technologies.

[0007] The technical solution of the present invention is as follows: This invention proposes a water-dispersible granule containing bispyribac-methyl, comprising the following raw materials in parts by weight: 50-60 parts of active ingredient, 6-8 parts of dispersant, 5-10 parts of disintegrant, 2-4 parts of wetting agent, 1-2 parts of defoamer, 2-4 parts of binder, and 10-12 parts of filler; wherein the active ingredient is composed of bispyribac-methyl and isoxazoline, including 2-cyclohexylaminoethanesulfonic acid and / or sulfonate.

[0008] As a further technical solution, the sulfonate includes one of dodecylbenzene sulfonate, hexadecylbenzene sulfonate, and octadecylbenzene sulfonate.

[0009] As a further technical solution, the sulfonate is hexadecylbenzene sulfonate.

[0010] As a further technical solution, the dispersant is composed of 2-cyclohexylaminoethanesulfonic acid and sulfonate.

[0011] As a further technical solution, the mass ratio of 2-cyclohexylaminoethanesulfonic acid to sulfonate is 1:3~5.

[0012] As a further technical solution, the mass ratio of 2-cyclohexylaminoethanesulfonic acid to sulfonate is 1:4.

[0013] In this invention, when the dispersant is composed of hexadecylbenzene sulfonate and 2-cyclohexylaminoethanesulfonic acid, it can better promote the disintegration and dispersion of water-dispersible granules in water, effectively block the mutual attraction between particles, prevent the aggregation of dispersed solid particles, maintain suspension and uniform dispersion in water, further improve the suspension rate and disintegration properties of water-dispersible particles, solve the problems of poor dispersion performance and slow disintegration rate of water-dispersible granules, improve the effect of active ingredients, reduce the amount of pesticides used, and has important significance for environmental protection.

[0014] As a further technical solution, the disintegrant includes one or more of sodium tripolyphosphate, sodium carboxymethyl starch, and silica.

[0015] As a further technical solution, the wetting agent includes one or two of polyethylene glycol and fatty alcohol polyvinyl ether.

[0016] As a further technical solution, the filler includes one or more of silica, kaolin, and diatomaceous earth.

[0017] As a further technical solution, the adhesive includes one or more of polyvinyl alcohol, polyvinylpyrrolidone, and xanthan gum.

[0018] As a further technical solution, the defoamer is an organosilicone defoamer.

[0019] The present invention also proposes a method for preparing water-dispersible granules containing diclofenac, comprising the following steps: pulverizing the raw material, adding water and mixing evenly, and then granulating to obtain water-dispersible granules.

[0020] The working principle and beneficial effects of this invention are as follows: In this invention, bispyribac-methyl and isoxaflutole are the main active ingredients, and dispersants, disintegrants, wetting agents, thickeners, defoamers, and fillers are added as excipients. The dispersant is 2-cyclohexylaminoethanesulfonic acid and / or sulfonate, which improves the dispersion performance and disintegration rate of the water-dispersible granules and effectively solves the problem that the effective active ingredients cannot play a good role and that the large-scale use of insecticides causes environmental pollution. Detailed Implementation

[0021] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0022] In the following embodiments and comparative examples: Polyvinyl alcohol: Model R1130, Kuraray, Japan; Polyvinylpyrrolidone: Model K60, Guangdong Yuemei Chemical Co., Ltd.; Defoamer: Model BYK141, Guangzhou Ruyi Chemical Co., Ltd.

[0023] Example 1 A method for preparing a water-dispersible granule containing bispyribac-methyl includes the following steps: 50 parts of active ingredient, 6 parts of dispersant, 5 parts of sodium tripolyphosphate, 2 parts of polyethylene glycol, 1 part of defoamer, 2 parts of polyvinyl alcohol, and 10 parts of kaolin were pulverized and mixed with 80 parts of water. The mixture was then spray-dried and granulated to obtain water-dispersible granules. The dispersant was hexadecylbenzene sulfonate, and the active ingredient consisted of bispyribac-methyl and isoxaflutole in a mass ratio of 1:1.

[0024] Example 2 A method for preparing a water-dispersible granule containing bispyribac-methyl includes the following steps: 55 parts of active ingredient, 7 parts of dispersant, 8 parts of fumed silica, 3 parts of fatty alcohol polyvinyl ether, 1.5 parts of defoamer, 3 parts of polyvinylpyrrolidone, and 11 parts of kaolin were pulverized and then mixed with 90 parts of water. The mixture was then spray-dried and granulated to obtain water-dispersible granules. The dispersant was hexadecylbenzene sulfonate, and the active ingredient consisted of bispyribac-methyl and isoxazoline in a mass ratio of 1:5.

[0025] Example 3 A method for preparing a water-dispersible granule containing bispyribac-methyl includes the following steps: 60 parts of active ingredient, 8 parts of dispersant, 10 parts of sodium tripolyphosphate, 4 parts of polyethylene glycol, 2 parts of defoamer, 4 parts of polyvinylpyrrolidone, and 12 parts of diatomaceous earth were pulverized and then mixed with 100 parts of water. The mixture was then spray-dried and granulated to obtain water-dispersible granules. The dispersant was hexadecylbenzene sulfonate, and the active ingredient consisted of bispyribac-methyl and isoxaflutole in a mass ratio of 1:6.

[0026] Example 4 The only difference between this embodiment and Example 1 is that the dispersant is 2-cyclohexylaminoethanesulfonic acid.

[0027] Example 5 The only difference between this embodiment and Example 1 is that the dispersant is octadecylbenzene sulfonate.

[0028] Example 6 The only difference between this embodiment and Example 1 is that the dispersant is dodecylbenzene sulfonate.

[0029] Example 7 The only difference between this embodiment and Example 1 is that the dispersant is composed of 2-cyclohexylaminoethanesulfonic acid and sodium hexadecyl sulfonate in a mass ratio of 1:2.

[0030] Example 8 The only difference between this embodiment and Example 1 is that the dispersant is composed of 2-cyclohexylaminoethanesulfonic acid and sodium hexadecyl sulfonate in a mass ratio of 1:3.

[0031] Example 9 The only difference between this embodiment and Example 1 is that the dispersant is composed of 2-cyclohexylaminoethanesulfonic acid and sodium hexadecyl sulfonate in a mass ratio of 1:4.

[0032] Example 10 The only difference between this embodiment and Example 1 is that the dispersant is composed of 2-cyclohexylaminoethanesulfonic acid and sodium hexadecyl sulfonate in a mass ratio of 1:5.

[0033] Example 11 The only difference between this embodiment and Example 1 is that the dispersant is composed of 2-cyclohexylaminoethanesulfonic acid and sodium hexadecyl sulfonate in a mass ratio of 1:6.

[0034] Example 12 The only difference between this embodiment and Example 1 is that the dispersant is composed of 2-cyclohexylaminoethanesulfonic acid and sodium dodecyl sulfonate in a mass ratio of 1:4.

[0035] Example 13 The only difference between this embodiment and Example 1 is that the dispersant is composed of 2-cyclohexylaminoethanesulfonic acid and sodium octadecyl sulfonate in a mass ratio of 1:4.

[0036] Comparative Example 1 The only difference between this comparative example and Example 1 is that the dispersant is sodium tripolyphosphate.

[0037] Test case The suspension rates of the water-dispersible granules prepared in Examples 1-13 and Comparative Example 1 were determined according to the determination method in CIPAC MT 184, and the results are shown in Table 1.

[0038] Table 1. Performance test results of water-dispersible granules in Examples 1-13 and Comparative Example 1

[0039] Compared with Example 1, Comparative Examples 1 and Examples 4-6 changed the dispersant. As a result, the suspension rate and disintegration of Examples 1 and Examples 4-6 were better than those of Comparative Example 1, indicating that 2-cyclohexylaminoethanesulfonic acid or sulfonate as dispersant can improve the suspension rate and disintegration of water-dispersible granules.

[0040] Compared with Examples 1 and 4-6, the dispersants in Examples 7-11 consisted of 2-cyclohexylaminoethanesulfonic acid and sulfonate. As a result, the suspension rate and disintegration of Examples 7-11 were better than those in Examples 1 and 4-6, indicating that when the dispersant consists of 2-cyclohexylaminoethanesulfonic acid and sulfonate, the suspension and disintegration of the water-dispersible granules can be further improved.

[0041] The suspension rate and disintegration properties of the water-dispersible granules in Examples 8-10 were superior to those in Examples 7 and 11, indicating that a mass ratio of sodium hexadecyl sulfonate to sulfonate of 1:3-5 can further improve the suspension and disintegration properties of the water-dispersible granules. Furthermore, analysis of Examples 12 and 13 shows that the dispersant composed of 2-cyclohexylaminoethanesulfonic acid and sodium hexadecyl sulfonate exhibits the best effect.

[0042] Experimental Example 2 Field control efficacy of isoxaflutole and diprotein (5:1) against cucumber aphids (1) Experimental setup: One experimental group and two control groups were set up. Experimental group: isoxazoline and bispyribac-methyl (5:1), i.e. bispyribac-methyl and isoxazoline in Example 2; Control group 1: Water-dispersible granules containing only isoxazoline at a mass fraction of 62%; Control group 2: Water-dispersible granules containing only 62% bispyribac-methyl.

[0043] (2) Experimental method: According to the experimentally designed dosage of pesticide, a backpack sprayer was used to spray the entire plant of each experimental plot evenly. Before application, 5 points were sampled in each plot, and 10 to 20 cucumber plants were sampled at each point and tagged (total number of plants). The number of adult and nymph aphids on each cucumber plant was investigated and recorded. The number of residual aphids was investigated on the 1st, 3rd and 7th day after application.

[0044] (3) Statistical analysis of experimental results Calculate the insect population reduction rate and control effectiveness using the following formula:

[0045] The calculation results are shown in Table 2.

[0046] Table 2. Field control efficacy of bispyribac-methyl and isoxazoline against aphids.

[0047] As can be seen from the table, compared with isoxaflutole in control group 1 and bispyribac-methyl in control group 2, the isoxaflutole:bispyribac-methyl ratio of 5:1 in the experimental group significantly improved the control effect on aphids at the experimental dosage, and the control effect increased with the increase of dosage. This indicates that the insecticidal composition of isoxaflutole and bispyribac-methyl is significantly more effective in controlling cucumber aphids than isoxaflutole and bispyribac-methyl alone.

[0048] Experimental Example 3 Field control efficacy of isoxaflutole and diprotein (1:1) against tomato whiteflies (1) Experimental setup: One experimental group and two control groups were set up. Experimental group: isoxazoline and bispyribac-methyl (1:1), i.e. isoxazoline and bispyribac-methyl from Example 1; Control group 1: Water-dispersible granules containing only isoxazoline with a mass fraction of 66.7%; Control group 2: Water-dispersible granules containing only 66.7% bispyribac-methyl.

[0049] (2) Experimental method: According to the designed experimental dosage, a backpack sprayer was used to spray the entire plant of each experimental plot evenly. Before application, 5 points were sampled in each plot, and 10 to 20 tomato plants were sampled at each point and tagged (total number of plants). The number of adult and nymph whiteflies on each tomato plant was investigated and recorded. The number of residual whiteflies was investigated on the 1st, 3rd, 5th, 7th and 10th days after application.

[0050] (3) Experimental results: The calculation formula is the same as that in Experiment 2, and the calculation results are shown in Table 3.

[0051] Table 3. Field control efficacy of isoxaflutole and diclofenac against whiteflies.

[0052] As can be seen from the table above, compared with isoxaflutole in control group 1 and bispyribac-methyl in control group 2, the experimental group's isoxaflutole:bispyribac-methyl (1:1) showed a significantly improved control effect on whiteflies at the experimental dosage, and the control effect increased with the increase of dosage. This indicates that the insecticidal combination of isoxaflutole and bispyribac-methyl is significantly more effective in controlling tomato whiteflies than isoxaflutole and bispyribac-methyl alone.

[0053] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A water-dispersible granule containing diprofen, characterized in that, The raw material comprises the following components in parts by weight: 50-60 parts active ingredient, 6-8 parts dispersant, 5-10 parts disintegrant, 2-4 parts wetting agent, 1-2 parts defoamer, 2-4 parts binder, and 10-12 parts filler; wherein the active ingredient is composed of bispyribac-methyl and isoxazoline, and the dispersant is composed of 2-cyclohexylaminoethanesulfonic acid and sulfonate in a mass ratio of 1:3-5; The sulfonate is hexadecylbenzene sulfonate; The disintegrant includes one or more of sodium tripolyphosphate, sodium carboxymethyl starch, and silica. The wetting agent includes one or two of polyethylene glycol and fatty alcohol polyvinyl ether; The filler includes one or more of silica, kaolin, and diatomaceous earth. The adhesive includes one or more of polyvinyl alcohol, polyvinylpyrrolidone, and xanthan gum.

2. The method for preparing a water-dispersible granule containing dipropionate according to claim 1, characterized in that, The process includes the following steps: after crushing the raw material, adding water and mixing it evenly, granulating it to obtain a water-dispersible granule.

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