CN112075442B - Water dispersible granule and preparation method thereof - Google Patents
Water dispersible granule and preparation method thereof Download PDFInfo
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- CN112075442B CN112075442B CN202010984043.3A CN202010984043A CN112075442B CN 112075442 B CN112075442 B CN 112075442B CN 202010984043 A CN202010984043 A CN 202010984043A CN 112075442 B CN112075442 B CN 112075442B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- 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
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- 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
- A01N47/40—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 a double or triple bond to nitrogen, e.g. cyanates, cyanamides
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Abstract
The application provides a water dispersible granule and a preparation method thereof. The water dispersible granule comprises 5-15 parts of emamectin benzoate, 20-40 parts of thiacloprid, 10-30 parts of azoxystrobin, 13-25 parts of dispersing agent, 2-4 parts of wetting agent, 0.5-2 parts of antioxidant, 5-10 parts of disintegrating aid and 0-20 parts of filler. The water dispersible granule reduces the generation probability of pesticide resistance of crop pests, enhances the insecticidal effect and reduces the insecticidal cost.
Description
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to a water dispersible granule and a preparation method thereof.
Background
Emamectin benzoate is abbreviated as emamectin benzoate, and emamectin benzoate mainly kills insects in a stomach poisoning and contact killing mode. The emamectin benzoate has very high activity for preventing and controlling lepidoptera, acarine, coleopteran and coleopteran pests, has the characteristics of biological pesticides with ultrahigh efficiency, low toxicity, low residue, no public nuisance and the like, and is widely used for preventing and controlling various pests on different crops such as vegetables, fruit trees, cotton and the like.
However, with the increase of the medication period, the drug resistance of pests to emamectin benzoate is increased year by year, and the insecticidal effect can be achieved by increasing the dosage and the medication frequency, so that the cost is increased, and the environmental pressure is increased.
Therefore, it is highly desirable to solve the problems that the resistance of pests to emamectin benzoate is increased to weaken the insecticidal effect and increase the insecticidal cost.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the water dispersible granule capable of reducing the generation probability of drug resistance, enhancing the insecticidal effect and reducing the insecticidal cost and the preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
the water dispersible granule comprises the following components in parts by mass:
in one embodiment, the dispersant is at least one of a polycarboxylate-type dispersant, a lignosulfonate-type dispersant, and a polynaphthalene formaldehyde sulfonate anion.
In one embodiment, the wetting agent is a sulfonate wetting agent.
In one embodiment, the antioxidant is at least one of PG, BHA, BHT and D902.
In one embodiment, the disintegration aid is at least one of anhydrous sodium sulphate, sodium citrate, potassium sulphate and ammonium sulphate.
In one embodiment, the filler is at least one of water-washed kaolin, light calcium carbonate, corn starch, white carbon black, and inert clay.
A preparation method of water dispersible granules comprises the following steps:
crushing emamectin benzoate, thiacloprid, azoxystrobin, a dispersing agent, a wetting agent, an antioxidant, a filler and an disintegration aid to obtain crushed materials;
mixing the crushed materials to obtain a mixture; and
and (3) performing granulation operation on the mixture to obtain the water dispersible granule.
In one embodiment, the particle size D98 of the crushed material is 10-15 μm.
In one embodiment, the mixing time for mixing the crushed materials is 8min to 20 min.
In one embodiment, the granulating operation on the mixture specifically includes the following steps:
extruding and granulating the mixture to obtain particles;
and drying the particles at the temperature of 60-80 ℃, and sieving to obtain the water dispersible granules.
Compared with the prior art, the invention has at least the following advantages:
1. in the water dispersible granule, emamectin benzoate, thiacloprid and azoxystrobin are used, wherein the emamectin benzoate and thiacloprid effectively prevent and treat basic insect pests, and the azoxystrobin effectively prevents and treats bacterial diseases;
2. in the water dispersible granule, the emamectin benzoate, thiacloprid and azoxystrobin are used in a combined manner, so that the effect of mutually promoting the insecticidal effect is achieved, the combined use of the emamectin benzoate, thiacloprid and azoxystrobin weakens the drug resistance of pests, the insecticidal using amount is reduced, the insecticidal cost is reduced, and the environmental pressure is reduced;
3. in the dispersible granule, the dispersing agent, the wetting agent and the antioxidant are used in a combined manner, so that the wetting effect and the dispersibility of the emamectin benzoate, the thiacloprid and the azoxystrobin are improved, the decomposition rate of the emamectin benzoate, the thiacloprid and the azoxystrobin in a mixing manner is reduced, and the compatibility of the emamectin benzoate, the thiacloprid and the azoxystrobin in a combined use manner is improved;
4. in the dispersible granule, the disintegrating aid and the filler are used, and the disintegrating aid and the filler are used together, so that the disintegrating speed and the dispersing speed of the dispersible granule are improved, and the dispersibility and the stability of the water dispersible granule are further improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a flow chart of steps of a preparation method of water dispersible granules in one embodiment of the invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The application provides a water dispersible granule. The water dispersible granule comprises the following components in parts by mass: 5-15 parts of emamectin benzoate; 20-40 parts of thiacloprid; 10-30 parts of azoxystrobin; 13-25 parts of a dispersing agent; 2-4 parts of a wetting agent; 0.5-2 parts of antioxidant; 5-10 parts of a disintegration aid; 0 to 20 portions of filler.
In the water dispersible granule, emamectin benzoate, thiacloprid, azoxystrobin, a dispersing agent, a wetting agent, an antioxidant, a disintegrating aid and a filler are used. The emamectin benzoate and the thiacloprid effectively prevent and treat basic insect pests, the azoxystrobin effectively prevents and treats bacterial diseases, and the emamectin benzoate, the thiacloprid and the azoxystrobin are used in a combined manner, so that the insect pests and diseases of crops are comprehensively prevented.
The combined use of the emamectin benzoate, the thiacloprid and the azoxystrobin has the effect of mutually promoting the insecticidal effect, and the combined use of the emamectin benzoate, the thiacloprid and the azoxystrobin weakens the drug resistance of pests, reduces the insecticidal using amount, reduces the insecticidal cost and simultaneously lightens the environmental pressure. The dispersant, the wetting agent and the antioxidant are used in a combined manner, so that the wetting effect and the dispersibility of the emamectin benzoate, the thiacloprid and the azoxystrobin are improved, the decomposition rate of the emamectin benzoate, the thiacloprid and the azoxystrobin in a mixing manner is reduced, and the compatibility of the emamectin benzoate, the thiacloprid and the azoxystrobin in the combined use is improved. The disintegrating aid and the filler are used and are used together, so that the disintegrating speed and the dispersing speed of the water dispersible granule are improved, and the dispersibility and the stability of the water dispersible granule are further improved.
In order to better understand the water dispersible granule, the water dispersible granule is further explained below, and the water dispersible granule of an embodiment comprises the following components in parts by mass: 5-15 parts of emamectin benzoate; 20-40 parts of thiacloprid; 10-30 parts of azoxystrobin; 13-25 parts of a dispersing agent; 2-4 parts of a wetting agent; 0.5-2 parts of antioxidant; 5-10 parts of a disintegration aid; 0 to 20 portions of filler.
In the water dispersible granule, emamectin benzoate, thiacloprid and azoxystrobin are used, wherein the emamectin benzoate and thiacloprid effectively prevent and treat basic insect pests, and the azoxystrobin effectively prevents and treats bacterial diseases, and the emamectin benzoate, the thiacloprid and the azoxystrobin are used in combination, so that the insect pests and diseases of crops are comprehensively prevented. The combined use of the emamectin benzoate, the thiacloprid and the azoxystrobin has the effect of mutually promoting the insecticidal effect, and the combined use of the emamectin benzoate, the thiacloprid and the azoxystrobin weakens the drug resistance of pests, reduces the insecticidal using amount, reduces the insecticidal cost and simultaneously lightens the environmental pressure. The dispersing agent improves the dispersion uniformity of the emamectin benzoate, the thiacloprid and the azoxystrobin, and avoids the problem of agglomeration of the emamectin benzoate, the thiacloprid and the azoxystrobin. The wetting agent reduces the surface tension or interfacial tension of emamectin benzoate, thiacloprid and azoxystrobin, so that solid materials are easier to wet, and the wetting agent has a better wetting effect on the emamectin benzoate, the thiacloprid and the azoxystrobin. The antioxidant reduces the decomposition rate of the emamectin benzoate and further improves the drug effect performance of the emamectin benzoate. The antioxidant, the dispersing agent and the wetting agent are used in a combined manner, so that the stability and the dispersion rate of the water dispersible granule are effectively improved, and the compatibility of the emamectin benzoate, thiacloprid and azoxystrobin in the combined use is further improved. The disintegrating aid and the filler are used together, so that the water dispersible granules can be disintegrated quickly to form a dispersion system with high suspension rate and high stability, and the dispersing efficiency of the water dispersible granules is improved.
The main effective components of emamectin benzoate, thiacloprid and azoxystrobin in the application are described in detail as follows:
emamectin benzoate (Emamectin benzoate), developed by Merck & Co of America, is a novel high-efficiency semi-synthetic antibiotic insecticide and acaricide synthesized by taking a fermentation product, namely, Abamectin B1, as a raw material. Its action mode is mainly stomach toxicity and contact poisoning, and has no systemic property for crops, but can be permeated into the epidermal tissue of crops, so that it possesses long effective period. The emamectin benzoate has very high activity for preventing and controlling lepidoptera, acarine, coleopteran and coleopteran pests, has the characteristics of biological pesticides with ultrahigh efficiency, low toxicity, low residue, no public nuisance and the like, and is widely used for preventing and controlling various pests on different crops such as vegetables, fruit trees, cotton and the like.
Thiacloprid (Thiacloprid) is a novel chloronicotinyl insecticide, which mainly acts on insect nerve postjunctional membranes, and is combined with a nicotine acetylcholine receptor to interfere normal conduction of insect nervous systems, so that nerve channel blockage is caused, a large amount of acetylcholine is accumulated, and the insects are excited abnormally and are killed by general spasm and paralysis. It has strong systemic, contact and stomach poisoning effects, has no cross resistance with conventional pyrethroid, carbamate and organophosphorus pesticides, and can be used for resistance control. Thiacloprid has good effect on pine moth, fall webworm, aphid, whitefly, various beetles and lepidoptera pests. Can be used for stem and leaf treatment and seed treatment, and has no mutual resistance when being mixed with other pesticide compounds.
Azoxystrobin (Azoxystrobin) is the first commercial Strobilurin fungicide developed successfully by Junda in 1992 and is effective against strains that are resistant to 1, 4-demethylase inhibitors, benzamides, dicarboxamides and benzimidazoles. Azoxystrobin can inhibit hypha growth and spore germination, and has a remarkable inhibitory effect on conidium production of fungi. The bactericidal composition is widely used for preventing and treating various diseases of economic crops due to high bactericidal activity, wide bactericidal spectrum, strong systemic property, safety to non-target crops and good compatibility with the environment.
It is to be noted that emamectin benzoate and thiacloprid can be used for controlling pests on crops such as fruit trees, vegetables, cotton, cereals and the like, but with the increase of the medication life, the drug resistance of the pests to the emamectin benzoate single agent and the thiacloprid single agent is enhanced year by year, and the insecticidal effect can be achieved only by increasing the dosage and the medication frequency, so that the cost is increased, and the environmental pressure is increased. The azoxystrobin is added into the emamectin benzoate and the thiacloprid, so that the safety of non-target crops is improved, the emamectin benzoate, the thiacloprid and the azoxystrobin have good compatibility with the environment, and the emamectin benzoate, the thiacloprid and the azoxystrobin are simultaneously applied, so that the growth influence of insect pests and diseases on the crops is reduced, namely, the emamectin benzoate, the thiacloprid and the azoxystrobin are jointly used, the application range of the pesticide is expanded, the generation probability of the drug resistance of the pests is reduced, the agricultural cost is also reduced, and the effect of preventing and controlling the insect pests is improved.
The water dispersible granules prepared from the emamectin benzoate, the thiacloprid and the azoxystrobin can avoid the dust flying problem of the emamectin benzoate, the thiacloprid and the azoxystrobin, further reduce the pollution to the environment, effectively improve the stability of effective components, increase the content ratio of the emamectin benzoate, the thiacloprid and the azoxystrobin by preparing the emamectin benzoate, the thiacloprid and the azoxystrobin into the water dispersible granules, reduce the volume of finished pesticides of the emamectin benzoate, the thiacloprid and the azoxystrobin, and save the packaging, storage and transportation costs.
It should also be noted that three insecticidal effective components, namely emamectin benzoate, thiacloprid and azoxystrobin, are added into the water dispersible granule simultaneously, so that the contact surface of the emamectin benzoate, thiacloprid and azoxystrobin in the water dispersible granule is increased, heat is easily generated in the process of preparing the water dispersible granule, and the compatibility of the emamectin benzoate, thiacloprid and azoxystrobin in the water dispersible granule is further damaged, so that the water dispersible granule cannot form a stable dispersion system, the insecticidal effect of the water dispersible granule is reduced, and the insecticidal cost is increased.
In one embodiment, the filler is 0.01-20 parts by weight. It can be understood that the filler is added into the emamectin benzoate, the thiacloprid and the azoxystrobin, so that the emamectin benzoate, the thiacloprid and the azoxystrobin can be quickly disintegrated, a dispersion system with high stability is promoted to be quickly formed, and the dispersion efficiency of the water dispersible granule is improved.
In one embodiment, the dispersant is at least one of a polycarboxylate dispersant, a lignosulfonate dispersant, and a naphthalene formaldehyde sulfonate anion. It can be understood that the hydrophobicity of the molecular main chain of the polycarboxylate dispersant, the hydrophilicity of the side chain and the existence of side chain active groups (methyl [ -CH 3], isobutyl [ -CCH 3], ester group [ -COOR ], phenyl [ -C6H 5]) play a certain role in steric stabilization on the emamectin benzoate, thiacloprid and azoxystrobin, so that the coagulation resistance among or among the emamectin benzoate, thiacloprid and azoxystrobin is increased; the dissociation of the lignosulfonate dispersant and the polynaphthalenesulfonate anion dispersant is negative, which is beneficial to mutual repulsion among emamectin benzoate, thiacloprid and azoxystrobin or between the emamectin benzoate, thiacloprid and azoxystrobin, and further increases the agglomeration resistance among the emamectin benzoate, thiacloprid and azoxystrobin, so that the polycarboxylate dispersant, the lignosulfonate dispersant and the naphthaldehyde sulfonate anion effectively prevent the agglomeration of the emamectin benzoate, thiacloprid and azoxystrobin, and further improves the dispersion stability of the emamectin benzoate, thiacloprid and azoxystrobin.
In one embodiment, the polycarboxylate type dispersant is at least one of SD-816, Tersperse2700, YUS-WG7, and D-518. It is understood that SD-816 mainly contains sodium polycarboxylate. Tersperse2700 has sodium polycarboxylate as a main component. The main component of YUS-WG7 is sodium polycarboxylate. The main component of D-518 is sodium polycarboxylate. SD-816, Tersperse2700, YUS-WG7 and D-518 play a certain role in steric stabilization of emamectin benzoate, thiacloprid and azoxystrobin, so that the coagulation resistance among or among the emamectin benzoate, thiacloprid and azoxystrobin is increased
In one embodiment, the lignosulfonate dispersant is at least one of Reax 907, Reax 910, lignin LX, Ultrazine NA, and Ufoxane 3A. It is understood that the main component of Reax 907 is sodium lignosulfonate. The main component of Reax 910 is sodium lignosulfonate. The main component of the lignin LX is sodium lignosulfonate. The main component of the Ultrazine NA is sodium lignosulfonate. The main component of the Ufoxane 3A is sodium lignosulfonate. Reax 907, Reax 910, lignin LX, Ultrazine NA and Ufoxane 3A are beneficial to mutual repulsion among emamectin benzoate, thiacloprid and azoxystrobin, so that the agglomeration of the emamectin benzoate, thiacloprid and azoxystrobin is effectively reduced, and the dispersion stability of the emamectin benzoate, thiacloprid and azoxystrobin is improved.
In one embodiment, the polynaphthalene sulfonate anion dispersant is polynaphthalene sulfonate anion 207K. The main component of the polynaphthalenesulfonate anion 207K is polynaphthalenesulfonate anion. It can be understood that the polynaphthalene formaldehyde sulfonate anion 207K does not cause dust flying in the using process, has less pollution to the safety of operators and the environment, and has better dispersing effect on emamectin benzoate, thiacloprid and azoxystrobin.
In one embodiment, the wetting agent is a sulfonate wetting agent. It can be understood that the sulfonate wetting agent reduces the surface tension of emamectin benzoate, thiacloprid and azoxystrobin, has better affinity adsorption effect on the emamectin benzoate, thiacloprid and azoxystrobin, improves the dispersion effect of the emamectin benzoate, thiacloprid and azoxystrobin, and further improves the dispersibility of the water dispersible granule.
In one embodiment, the sulfonate wetting agent is at least one of YUS-SXC, W-610, L-WET/P, Terwet1004, YKW-18011, and sodium dodecyl sulfate. It is understood that the main component of YUS-SXC is C10-C14Alkyl derivative benzenesulfonic acid sodium salt. Master of W-610The essential component is C14～C16Sodium alkenyl sulfonate. The main component of the L-WET/P is alkyl sulfonate. Terwet1004 is based on alkyl aryl sulfonate. The main component of YKW-18011 is alkyl aryl sulfonate. The YUS-SXC, W-610, L-WET/P, Terwet1004, YKW-18011 and sodium dodecyl sulfate have good wetting effects on emamectin benzoate, thiacloprid and azoxystrobin, the dispersing effects of the emamectin benzoate, the thiacloprid and the azoxystrobin are improved, and the dispersibility of the water dispersible granules is further improved.
It is understood that, as the content of the active ingredients of the pesticide preparation increases, the wetting effect of the conventional wetting agent cannot meet the dispersion requirement of the water dispersible granule containing the emamectin benzoate, the thiacloprid and the azoxystrobin, and therefore, in order to improve the dispersion effect of the water dispersible granule containing the emamectin benzoate, the thiacloprid and the azoxystrobin, in one embodiment, the sulfonate wetting agent comprises alkyl sulfonate. It can be understood that the carbon chain of the alkyl sulfonate has a good affinity coating effect on the emamectin benzoate, the thiacloprid and the azoxystrobin, so that the emamectin benzoate, the thiacloprid and the azoxystrobin can be stably adsorbed in the carbon chain, and the dispersibility of the emamectin benzoate, the thiacloprid and the azoxystrobin is improved.
Further, the sulfonate wetting agents include alkylarenesulfonates. It can be understood that the alkyl aromatic sulfonate contains a benzene ring, and the carbon chain structure of the benzene ring enables the alkyl aromatic sulfonate to have a better affinity coating effect on the emamectin benzoate, the thiacloprid and the azoxystrobin, so that the emamectin benzoate, the thiacloprid and the azoxystrobin are more stably adsorbed in the carbon chain, and the dispersibility of the emamectin benzoate, the thiacloprid and the azoxystrobin is improved.
In one embodiment, the sulfonate wetting agent comprises C10～C14The alkyl derivative benzenesulfonate of (1). It can be understood that the carbon chain length of the sulfonate wetting agent plays a critical role in the wetting effect of the raw emamectin benzoate, the azoxystrobin and the thiacloprid, and for the particle size range of the water dispersible granule, the excessively long or short carbon chain of the sulfonate wetting agent can influence the adsorbability of the emamectin benzoate, the azoxystrobin and the thiacloprid, and when the sulfonate wetting agent is C10～C14Alkyl derivatives ofWhen it is benzene sulfonate, C10～C14The alkyl derivative benzenesulfonate has stable adsorption performance on emamectin benzoate, azoxystrobin and thiacloprid, so that the emamectin benzoate, azoxystrobin and thiacloprid have good stability under the conditions of mixing, stirring, drying or other external conditions with large changes, and the suspension rate of the water dispersible granule containing the emamectin benzoate, azoxystrobin and thiacloprid is further improved.
In one of the embodiments, the antioxidant is at least one of PG, BHA, BHT and D902. The PG contains propyl gallate as main component. The main component of BHA is butylated hydroxyanisole. BHT is mainly composed of 2, 6-di-tert-butyl-4-methylphenol. The main components of D902 are butyl hydroxy anisole and potassium polyphosphate. D902 has excellent compatibility with emamectin benzoate, has better anti-decomposition effect on the emamectin benzoate, reduces the decomposition rate of the emamectin benzoate, and further improves the stability and the pharmacodynamic performance of the water dispersible granule; PG, BHA and BHT are helpful for reducing the decomposition rate of emamectin benzoate, and further effectively improve the stability and the pharmacodynamic property of the water dispersible granule.
In one embodiment, the disintegration aid is at least one of anhydrous sodium sulphate, sodium citrate, potassium sulphate and ammonium sulphate. The main component of anhydrous sodium sulfate is anhydrous sodium sulfate. The anhydrous sodium sulphate, the sodium citrate, the potassium sulfate and the ammonium sulfate are beneficial to eliminating the binding force inside each water dispersible granule of the water dispersible granule in the granulation process, the disintegration speed of the water dispersible granule is improved, the water dispersible granule is further promoted to form a stable dispersion system, and the speed of the water dispersible granule forming the stable dispersion system is improved.
In one embodiment, the filler is at least one of water-washed kaolin, light calcium carbonate, corn starch, white carbon black, and inert clay. It can be understood that the shrinkage of the water dispersible granule is reduced and the stability of the water dispersible granule is improved by washing kaolin, light calcium carbonate, corn starch, white carbon black and inert clay, and the light stability and the corrosion resistance of the water dispersible granule are improved.
The application also provides a preparation method of the water dispersible granule. The preparation method of the water dispersible granule comprises the following steps: crushing emamectin benzoate, thiacloprid, azoxystrobin, a dispersing agent, a wetting agent, an antioxidant, a filler and an disintegration aid to obtain crushed materials; mixing the crushed materials to obtain a mixture; and (4) granulating the mixture to obtain the water dispersible granule.
In the preparation method of the water dispersible granule, emamectin benzoate, thiacloprid, azoxystrobin, a dispersing agent, a wetting agent, an antioxidant and a disintegrating aid are crushed. It can be understood that the addition of the antioxidant reduces the thermal decomposition rate of the emamectin benzoate, the thiacloprid and the azoxystrobin when the emamectin benzoate is mixed, and the addition of the dispersing agent, the wetting agent, the filler and the disintegration aid improves the dispersibility and stability of the emamectin benzoate, the thiacloprid and the azoxystrobin and avoids the problem of agglomeration of the emamectin benzoate, the thiacloprid and the azoxystrobin. It can also be understood that in the process of crushing emamectin benzoate, thiacloprid and azoxystrobin, the contact among emamectin benzoate, thiacloprid and azoxystrobin is increased, so that heat is generated, the drug effect of emamectin benzoate is reduced, the compatibility of emamectin benzoate, thiacloprid and azoxystrobin in the dispersible granules is damaged, so that the water dispersible granules cannot form a stable dispersion system, the insecticidal effect of the water dispersible granules is reduced, and the insecticidal cost is increased.
In order to better understand the preparation method of the water dispersible granule, the following further explains the preparation method of the water dispersible granule, and please refer to fig. 1, the preparation method of the water dispersible granule of an embodiment includes the following steps:
s100, crushing emamectin benzoate, thiacloprid, azoxystrobin, a dispersing agent, a wetting agent, an antioxidant and an disintegration aid to obtain crushed materials. It can be understood that, when the emamectin benzoate, the thiacloprid, the azoxystrobin, the dispersing agent, the wetting agent, the antioxidant and the disintegration aid are crushed, a large amount of mechanical energy is converted into heat energy, so that the decomposition rate of the emamectin benzoate is increased, the effective content of the emamectin benzoate is reduced, and therefore, the antioxidant is added firstly and then the crushing operation is carried out, so that the antioxidant firstly protects the emamectin benzoate, and the decomposition rate of the emamectin benzoate in the crushing process is reduced. The water dispersible granule can be prepared by adding the dispersing agent and the wetting agent disintegration aid, and then crushing, so that the problems that the contact surface of the emamectin benzoate, the thiacloprid and the azoxystrobin is increased, heat is generated in the process of preparing the water dispersible granule, and the compatibility of the emamectin benzoate, the thiacloprid and the azoxystrobin in the water dispersible granule is damaged, so that the water dispersible granule cannot form a stable dispersion system, namely, the emamectin benzoate, the thiacloprid and the azoxystrobin are coagulated in the crushing process, the insecticidal effect of the water dispersible granule is reduced, the insecticidal cost is increased, the dispersibility and the stability of the water dispersible granule are improved, the insecticidal effect of the water dispersible granule is improved, and the insecticidal cost is reduced.
And S200, mixing the crushed materials to obtain a mixture. It can be understood that the mixture is mixed, so that the dispersibility of the emamectin benzoate, the thiacloprid and the azoxystrobin is improved, and the subsequent granulation operation is favorably and smoothly carried out.
S300, performing granulation operation on the mixture to obtain the water dispersible granule. It can be understood that the mixture is granulated, so that the adhesiveness and the cohesiveness of the water dispersible granule are weakened, and the fluidity of the mixture before granulation is obviously improved. And the granulation operation of the mixture is beneficial to reducing the segregation phenomenon of the granularity and the density of each component of the mixture, improving the dispersion stability of the emamectin benzoate, the thiacloprid and the azoxystrobin, preventing dust from flying and adhesion on the wall of the device, and reducing the loss of the emamectin benzoate, the thiacloprid and the azoxystrobin in the storage and transportation processes.
In one embodiment, before the crushing operation, the method further comprises the following steps: the emamectin benzoate, thiacloprid, azoxystrobin, dispersing agent, wetting agent, antioxidant and disintegration aid are subjected to primary mixing operation, so that the uniform dispersion degree of the emamectin benzoate, thiacloprid, azoxystrobin, dispersing agent, wetting agent, antioxidant and disintegration aid in crushing operation is improved, the decomposition rate of the emamectin benzoate is reduced, and the pharmacodynamic performance, the dispersing performance and the stability of the water dispersible granule are improved.
In one embodiment, the particle size D98 of the pulverized material is 10 μm to 15 μm. The particle size D98 of the pulverized material of 10 to 15 μm means that the number of particles having a particle size of 10 to 15 μm in the pulverized material accounts for 98% of the total number of particles. It can be understood that the particle size D98 of the crushed material is 10-15 μm, and the dispersibility and stability of the water dispersible granule are improved on the premise of keeping lower energy consumption.
In one embodiment, the mixing time for mixing the crushed materials is 8-20 min, so that the dispersity of the crushed materials is ensured on the premise of keeping low energy consumption.
In one embodiment, the granulation of the mixture specifically comprises the steps of: extruding and granulating the mixture to obtain particles; and drying and sieving the particles at the temperature of 60-80 ℃ to obtain the water dispersible granules. It can be understood that too low drying temperature easily causes too high water content of a sample and poor stability, and too high drying temperature easily causes the sample to be difficult to disintegrate, and has low suspension percentage and poor dispersibility, so that the particles are dried and sieved at 60-80 ℃ to obtain the water dispersible granule, so that the water dispersible granule has better stability, dispersibility and suspension percentage.
Some specific examples are listed below, and if mentioned%, all are expressed in weight percent. It should be noted that the following examples are not intended to be exhaustive of all possible cases, and that the materials used in the following examples are commercially available without specific recitation.
Example 1
1kg of emamectin benzoate; 3kg thiacloprid; 2kg azoxystrobin; 0.5kg 207K; 0.4kg 2700; 0.8kg of Ufoxane 3A; 0.2kg of YUS-SXC; 0.7kg of anhydrous sodium sulfate; 0.05kg D902; 1.35kg of corn starch.
Example 2
1kg of emamectin benzoate; 3kg thiacloprid; 2kg azoxystrobin; 0.5kg 207K; 0.8kgUfoxane 3A; 0.2kg of YUS-SXC; 0.7kg of anhydrous sodium sulfate; 0.05kg D902; 1.75kg of corn starch.
Example 3
1kg of emamectin benzoate; 3kg thiacloprid; 2kg azoxystrobin; 0.5kg 207K; 0.2kg 2700; 0.8kgUfoxane 3A; 0.2kg of YUS-SXC; 0.7kg of anhydrous sodium sulfate; 0.05kg D902; 1.55kg of corn starch.
Example 4
1kg of emamectin benzoate; 3kg thiacloprid; 2kg azoxystrobin; 0.5kg D500; 0.2kg 2700; 0.8kg of Ufoxane 3A; 0.2kg of YUS-SXC; 0.7kg of anhydrous sodium sulfate; 0.1kg BHT; 1.5kg of corn starch.
Example 5
1kg of emamectin benzoate; 3kg thiacloprid; 2kg azoxystrobin; 0.8kg of D500; 0.2kg 2700; 0.8kg lignin LX; 0.2kg of YUS-SXC; 0.7kg of anhydrous sodium sulfate; 0.1kg BHT; 1.2kg of corn starch.
Example 6
1kg of emamectin benzoate; 3kg thiacloprid; 2kg azoxystrobin; 0.8kg of D500; 0.2kg 2700; 0.8kg lignin LX; 0.2 kgYUS-SXC; 0.7kg of potassium sulfate; 0.1kg BHT; 1.2kg of corn starch.
Example 7
1kg of emamectin benzoate; 3kg thiacloprid; 2kg azoxystrobin; 0.8kg of D500; 0.2kg 2700; 0.8kg lignin LX; 0.2kg of YUS-SXC; 0.7kg of potassium sulfate; 0.1kg BHA; 1.2kg of kaolin.
Example 8
1kg of emamectin benzoate; 3kg thiacloprid; 2kg azoxystrobin; 0.8kg D500; 0.2kg 2700; 0.8kg lignin LX; 0.2kg of YUS-SXC; 0.7kg of potassium sulfate; 0.1kg BHA; 1.2kg of light calcium carbonate.
Example 9
0.5kg emamectin benzoate; 2.3kg thiacloprid; 3kg azoxystrobin; 0.5kg 207K; 0.4kg 2700; 0.4kg of Ufoxane 3A; 0.3kg of YUS-SXC; 0.5kg of anhydrous sodium sulfate; 0.1kg of D902; 2kg of corn starch.
Example 10
0.9kg emamectin benzoate; 4kg thiacloprid; 1kg azoxystrobin; 1kg 207K; 0.7kg 2700; 0.8kgUfoxane 3A; 0.4kg YUS-SXC; 1kg of anhydrous sodium sulfate; 0.2kg of D902.
Example 11
1.5kg emamectin benzoate; 2kg thiacloprid; 3kg azoxystrobin; 0.5kg 207K; 0.4kg 2700; 0.4kg of Ufoxane 3A; 0.3kg of YUS-SXC; 0.5kg of anhydrous sodium sulfate; 0.05kg D902; 1.35kg of corn starch.
Example 12
Crushing emamectin benzoate, thiacloprid, azoxystrobin, a dispersing agent, a wetting agent, an antioxidant, a filler and an disintegration aid to obtain a crushed material with the particle size D98 of 10 mu m;
mixing the pulverized materials for 20min to obtain a mixture; and
adding water to the mixture for humidification, and carrying out extrusion granulation to obtain particles;
and (3) drying the particles at the temperature of 80 ℃, and sieving to obtain the water dispersible granules with the water content of 2.31%.
Example 13
Crushing emamectin benzoate, thiacloprid, azoxystrobin, a dispersing agent, a wetting agent, an antioxidant, a filler and an disintegration aid to obtain a crushed material with the particle size D98 of 12 mu m;
mixing the pulverized materials for 15min to obtain a mixture; and
adding water to the mixture for humidification, and carrying out extrusion granulation to obtain particles;
and (3) drying and sieving the particles at 70 ℃ to obtain the water dispersible granules with the water content of 2.61%.
Example 14
Crushing emamectin benzoate, thiacloprid, azoxystrobin, a dispersing agent, a wetting agent, an antioxidant, a filler and an disintegration aid to obtain a crushed material with the particle size D98 of 15 microns;
mixing the pulverized materials for 8min to obtain a mixture; and
adding water to the mixture for humidification, and carrying out extrusion granulation to obtain particles;
and (3) drying the particles at the temperature of 60 ℃, and sieving to obtain the water dispersible granules with the water content of 2.86%.
The water dispersible granules prepared by the preparation method of the water dispersible granules are tested as follows.
Test 1
Purpose of the experiment
By using the preparation method of the water dispersible granule, five water dispersible granules with different pesticide active ingredients are prepared, and insect pest control effect tests are carried out on the water dispersible granules with the five different pesticide active ingredients prepared by using the preparation method of the water dispersible granule.
Test grouping
Test groups: the effective components of the pesticide in the test group are emamectin benzoate, thiacloprid and azoxystrobin;
comparison group: the effective component of the pesticide in the comparison group 1 is emamectin benzoate; the effective component of the pesticide in the comparison group 2 is thiacloprid; the effective components of the pesticide in the comparison group 3 are emamectin benzoate and thiacloprid; the effective components of the pesticide in the comparison group 4 are emamectin benzoate and azoxystrobin; the effective components of the pesticide in the comparison group 5 are thiacloprid and azoxystrobin.
Grouping farmland test areas: the farmland insect pest large area in the same place is divided into six test areas, namely an area 1, an area 2, an area 3, an area 4, an area 5 and an area 6.
It is to be noted that both the test and each comparative group contained dispersant D500, 2700 and lignin LX, wetting agent YUS-SXC, disintegrating aid potassium sulfate, antioxidant BHA and filler kaolin.
The test method comprises the following steps: by using the preparation method of the water dispersible granule, the water dispersible granules with different pesticide effective ingredients are prepared for the formulas of the test group and the comparison group respectively to obtain the water dispersible granules with different pesticide effective ingredients, and the field insecticidal effect of the water dispersible granules with different pesticide effective ingredients is detected.
Table 1 shows the amounts of each substance added in the test group and the comparative group.
Table 1: the addition amounts of the respective substances of the test group and the comparative group
The five groups of water dispersible granules with different pesticide active ingredients obtained in the test 1 are respectively tested for the actual field pest control effect in different farmland pest areas in the same place, and the number of the surviving pests is counted after three days, and the reduction rate and the control efficiency of the pests are calculated. The formulas for calculating the population reduction rate and the prevention and treatment efficiency are as follows:
the oral cavity decline rate (%) (number of pre-drug insects-number of post-drug insects)/number of pre-drug insects × 100;
control effect (%) - (oral cavity decline rate in control area-oral cavity decline rate in control area)/(oral cavity decline rate in control area) x 100
And (3) test results: the results of the test data of the test groups and the comparative groups 1 to 5 are shown in table 2:
table 2: test data results of test group and comparative group 1-5
As can be seen from Table 2, the difference between the control effect data of the test group and the control groups 1, 2, 4 and 5 is larger than that of the test group, which shows that the emamectin benzoate, thiacloprid and azoxystrobin have mutually promoted insecticidal effect when used in combination.
The water dispersible granules of examples 1 to 11 prepared by the method for preparing water dispersible granules of example 13 were tested as follows.
Test 2
Purpose of the experiment
The water dispersible granules of examples 15 to 25, namely the water dispersible granules of examples 1 to 11, prepared by the method for preparing the water dispersible granules of example 13 were tested for each performance.
Test grouping
Test groups: the water dispersible granules of examples 15 to 25 are prepared by the preparation method of the water dispersible granules of example 13;
in examples 15 to 25, the addition amounts of the respective substances in the actual production process are shown, and the data of examples 1 to 11 are converted into the addition amounts of the respective substances in the laboratory test, specifically, examples 1 to 11 correspond to examples 15 to 25 one by one.
Table 3 shows the addition amounts of the components of the water dispersible granule of examples 15-25:
table 3: the addition amount of each component of the water dispersible granule of example 15-25
The test method comprises the following steps: the water dispersible granules of examples 15-25 prepared by the preparation method of the water dispersible granule are respectively subjected to detection of suspension rate, decomposition rate, disintegration time and wetting time.
Test results
Table 4 shows the performance detection data of the water dispersible granules of examples 15-25:
table 4: data for detecting each property of the water dispersible granule of examples 15 to 25
Conclusion of the experiment
1. As can be seen from table 4, the water dispersible granules of examples 15 to 25 prepared by the preparation method of the water dispersible granule of example 13 all have good disintegration speed, wetting effect and suspension rate, and the decomposition rates of emamectin benzoate, thiacloprid and azoxystrobin are all low.
2. From table 4, it can be seen that the water dispersible granules of examples 15 to 25, namely the water dispersible granules of examples 1 to 11, prepared by the preparation method of the water dispersible granules of example 13 have improved suspension percentage of the water dispersible granules 2700.
3. From tables 3 and 4, it can be seen that in the water dispersible granule of example 18, that is, the water dispersible granule of example 4, D500 better improves the suspension rate of the water dispersible granule, the D500 effect is better than 207K, and BHT effectively reduces the decomposition rate of the emamectin benzoate.
4. As can be seen from tables 3 and 4, in the water dispersible granule of example 19, that is, the water dispersible granule of example 5, the amount of D500 is increased and the dispersant is replaced by lignin LX, so that the suspension percentage of the water dispersible granule is better improved.
5. As can be seen from tables 3 and 4, in the water dispersible granules of examples 20 to 22, that is, the water dispersible granules of examples 6 to 8, the disintegrating aid is replaced by anhydrous sodium sulfate, so that the disintegrating speed and the disintegrating effect are better improved, and the dissolution resistance of the emamectin benzoate is improved by BHA.
The water dispersible granule of example 7 was examined as follows.
Test 3
Purpose of the experiment
The water dispersible granules of examples 7-1 to 7-3 obtained at different drying operation temperatures in the preparation method of the water dispersible granule by using the test method were subjected to various performance tests, and the optimum drying operation temperature was selected.
Test method
The test method comprises the following steps: crushing emamectin benzoate, thiacloprid, azoxystrobin, a dispersing agent, a wetting agent, an antioxidant, a filler and an disintegration aid to obtain a crushed material with the particle size D98 of 10 mu m;
mixing the pulverized materials for 20min to obtain a mixture; and
adding water to the mixture for humidification, and carrying out extrusion granulation to obtain particles;
and (3) drying the particles at the temperature of X ℃, and sieving to obtain the water dispersible granules with the water content of 1%.
Note that X ℃ is 60 ℃, 70 ℃, 80 ℃, 90 ℃ and 100 ℃, respectively.
Test grouping
Test groups: the water dispersible granules of example 7-1, example 7-2, example 7-3, example 7-4 and example 7-5, which have the same composition and content as the water dispersible granules of example 21, respectively, obtained by the above test method;
control group: the composition and content of the water dispersible granule of the control group are shown in table 4:
table 4: composition components and content of water dispersible granules of control group
Test results
The data of the performance test of the water dispersible granule of the embodiment 7-1 to 7-3 are shown in the following table 5:
table 5: water dispersible granule of examples 7-1 to 7-5 and comparative examples 1 to 3 has various performance properties
Conclusion of the experiment
1. As can be seen from Table 5, the suspension percentage of the water dispersible granules of examples 7-1 to 7-5 is reduced when the temperature of the drying operation is increased to 90 ℃, and is obviously reduced when the temperature of the drying operation is increased to 100 ℃; the suspension rate of the water dispersible granules of comparative examples 1-3 is obviously reduced when the temperature of the drying operation is increased to 90 ℃. The water dispersible granule of example 7 is more excellent in heat resistance.
2. As can be seen from Table 5, the water dispersible granules of examples 7-1 to 7-5 have a preferable suspension percentage, water content and disintegration time at a drying temperature of 60 ℃ to 80 ℃.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (7)
1. The water dispersible granule is characterized by comprising the following components in parts by mass:
wherein the wetting agent is a sulfonate wetting agentWetting agents of the sulfonate type include C10～C14Alkyl derivative benzenesulfonate of (a);
the dispersant is at least one of polycarboxylate dispersant, lignosulfonate dispersant and polynaphthalene formaldehyde sulfonate anion;
the filler is at least one of washing kaolin, light calcium carbonate, corn starch, white carbon black and inert clay.
2. The water dispersible granule according to claim 1, wherein the antioxidant is at least one of PG, BHA, BHT and D902.
3. The water dispersible granule according to claim 1, wherein the disintegration aid is at least one of anhydrous sodium sulphate, sodium citrate, potassium sulphate and ammonium sulphate.
4. A preparation method of water dispersible granules, which is used for preparing the water dispersible granules of any one of claims 1 to 3 and comprises the following steps:
crushing emamectin benzoate, thiacloprid, azoxystrobin, a dispersing agent, a wetting agent, an antioxidant, a filler and an disintegration aid to obtain crushed materials;
mixing the crushed materials to obtain a mixture; and
and (3) performing granulation operation on the mixture to obtain the water dispersible granule.
5. The method for producing water dispersible granules according to claim 4, wherein the particle size D98 of the pulverized material is 10 to 15 μm.
6. The method for producing water dispersible granules according to claim 4, wherein the mixing time for mixing the pulverized material is 8 to 20 min.
7. The preparation method of water dispersible granules according to claim 4, wherein the granulating operation of the mixture specifically comprises the following steps:
extruding and granulating the mixture to obtain particles;
and drying the particles at the temperature of 60-80 ℃, and sieving to obtain the water dispersible granules.
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| CN101305732A (en) * | 2007-12-27 | 2008-11-19 | 天津市兴光农药厂 | Pesticide combination containing thiacloprid |
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Denomination of invention: Water dispersible granule and its preparation method Effective date of registration: 20221205 Granted publication date: 20220510 Pledgee: China Co. truction Bank Corp Huizhou branch Pledgor: HUIZHOU YINNONG TECHNOLOGY Co.,Ltd. Registration number: Y2022980024525 |