CN108902158B - Suspending agent containing pyraclostrobin composition and application thereof - Google Patents

Suspending agent containing pyraclostrobin composition and application thereof Download PDF

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CN108902158B
CN108902158B CN201810940138.8A CN201810940138A CN108902158B CN 108902158 B CN108902158 B CN 108902158B CN 201810940138 A CN201810940138 A CN 201810940138A CN 108902158 B CN108902158 B CN 108902158B
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water
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CN108902158A (en
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丑靖宇
张国生
宋玉泉
米双
李天一
刘少武
遇璐
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Shenyang Sinochem Agrochemicals R&D Co Ltd
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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
    • A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
    • 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
    • A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • 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
    • A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/06—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings
    • A01N43/12—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings condensed with a carbocyclic ring
    • 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
    • A01N43/58—1,2-Diazines; Hydrogenated 1,2-diazines
    • 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
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/74—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
    • A01N43/76—1,3-Oxazoles; Hydrogenated 1,3-oxazoles

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention belongs to the field of agricultural acaricides, and relates to an aqueous suspension agent taking an active ingredient A and an active ingredient B as acaricide active ingredients and application thereof. The suspending agent containing the composition of the pyraclonil comprises active ingredients A and B as effective active ingredients, and is composed of 5-70 wt% of the active ingredients, 1-50 wt% of a dispersing agent, 0.5-5 wt% of a wetting agent, 0.5-8 wt% of a thickening agent, 0.1-2 wt% of an antifoaming agent, 1-20 wt% of an antifreezing agent, and the balance of water; wherein the active component A is ethiprole, the active component B is selected from pyridaben, spirodiclofen or etoxazole, and the weight ratio of the active component A to the active component B is 1: 20-20: 1. The acaricide composition has remarkable synergism, is safe to crops, accords with the national policy of reducing the application of pesticides and improving the efficiency, and is an ideal acaricide variety for preventing and treating pest mites at present.

Description

Suspending agent containing pyraclostrobin composition and application thereof
Technical Field
The invention belongs to the field of pesticide acaricide, and relates to a suspending agent containing an ethiprole composition and application thereof.
Background
It is known that acaricides have a remarkable effect on controlling agricultural and forestry pest mites or urban sanitary pest mites. In recent years, with the increasing requirements of people on environment and health, the use guidelines of pesticides are promoted to be developed towards the direction of reducing application and improving efficiency. The quality of the pesticide formulation and the preparation is a key factor for determining the effect and the value of the pesticide product, and if the best effect is required to be endowed to the active ingredients, the selection of an auxiliary agent system matched with the active ingredients and the dosage are particularly important. At present, a plurality of suspending agents containing the composition containing the pyrazoxynil are reported, and mainly comprise the following components:
the composition of the pyrazotoconazole and the spirodiclofen comprises the following components in percentage by weight: CN 104663668B discloses that the weight ratio of the two is 1: 20-20: 1, and the two can be used for preparing suspending agents, aqueous emulsion, water dispersible granules and other dosage forms; CN 106605657A discloses a mixed solution of the two in a weight ratio of 20: 1-1: 20: can be prepared into wettable powder, water dispersible granules, suspending agents, suspoemulsion, emulsion in water, microemulsion, microcapsule suspending agents or microcapsule suspension-suspending agents. CN 106035341A discloses that the weight ratio of the two is 50: 1-1: 50, and suspending agents, water dispersible granules and the like can be prepared.
The composition of the pyrazoxynil and the pyridaben comprises the following components in percentage by weight: CN 106605654A discloses that the weight ratio of the two is 1: 20-20: 1, and suspending agents, water dispersible granules and the like can be prepared. CN 105394044A discloses that the weight ratio of the two is 1: 40-50: 1, and the two can be prepared into suspending agents, water dispersible granules and the like. CN 104663666B discloses that the two can be prepared into suspending agent, aqueous emulsion, water dispersible granule and other dosage forms with the weight ratio of 1: 20-20: 1.
The composition of the pyrazotoconazole and the etoxazole comprises the following components in percentage by weight: CN 106417321A discloses that the weight ratio of the two is 1: 20-30: 1, and suspending agents, water dispersible granules and the like can be prepared. CN 104663672B discloses that the weight ratio of the two is 1: 20-20: 1, and the two can be used for preparing suspending agents, aqueous emulsion, water dispersible granules and other dosage forms.
Although the prior art shows that: the fenacet and spirodiclofen/pyridaben/etoxazole compound acaricide composition has obvious synergistic action, and the lasting time is obviously longer than that of a single agent. However, the acaricidal biological activity of the suspension agent product prepared by the prior art is comparable to or slightly higher than that of a corresponding original drug with the same dose, but no relevant report about the selection of a matching auxiliary agent system and the proportion of active components in a specific dosage form exists at present.
Disclosure of Invention
The invention aims to provide the suspending agent containing the pyrazoxyfen-ethyl composition and the application thereof, wherein the suspending agent has the advantages of reasonable components, obvious synergism, good acaricidal effect, low medication cost and safety to crops.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the suspending agent containing the composition of the pyraclonil comprises active ingredients A and B as effective active ingredients, and is composed of 5-70 wt% of the active ingredients, 1-50 wt% of a dispersing agent, 0.5-5 wt% of a wetting agent, 0.5-8 wt% of a thickening agent, 0.1-2 wt% of an antifoaming agent, 1-20 wt% of an antifreezing agent, and the balance of water; wherein the active component A is ethiprole, the active component B is selected from pyridaben, spirodiclofen or etoxazole, and the weight ratio of the active component A to the active component B is 1: 20-20: 1.
Preferably: the suspending agent comprises 5-70 wt% of active components, 1-50 wt% of dispersing agents, 0.5-5 wt% of wetting agents, 0.5-8 wt% of thickening agents, 0.1-2 wt% of defoaming agents, 1-20 wt% of antifreezing agents and the balance of water; wherein the active component A is ethiprole, the active component B is selected from pyridaben, spirodiclofen or etoxazole, and the weight ratio of the active component A to the active component B is 1: 10-10: 1.
Preferably, the suspending agent comprises 5-70 wt% of active components, 1-50 wt% of dispersing agent, 0.5-5 wt% of wetting agent, 0.5-8 wt% of thickening agent, 0.1-2 wt% of defoaming agent, 1-20 wt% of antifreezing agent and the balance of water; wherein the active component A is ethiprole, the active component B is selected from pyridaben, spirodiclofen or etoxazole, and the weight ratio of the active component A to the active component B is 1: 5-5: 1.
The dispersant may be selected from: sodium polyacrylate (SD-811), polycarboxylate (SD816, SD819, Emulson TRN14105, SP-2750, GY-D800, ULTRASURF 7023A, DURAMAXTMD-205 or DURAMAXTMD-305), carboxylate (SD815, SK-25CH or TANEMULL DA2880), carboxylic acid polymer copolymer (Atlox 4913), sulfonate (SK-20TX, SK-24R), aryl ether phosphate (SK-33SC), gemini amphiphilic surfactant complex (SP-SC3 or SP-SC29), natural polymer modifier (Lamfix SO), complexing auxiliary agent of polyacrylate copolymer (FS981), special structure polymer surfactant (SP-27001), EO/PO block polyether (D800 or Atlas G5000), block copolymer (TENSIFIX DB08, Tensiofix 303 or Tensiofix XA265), polymer surfactant with "ABA" regular structure (SP-2836), TWEEN L1505-LQ- (AP), TWEEN L5-LQ- (AP), TWEEN L1010-LQ- (AP); AP), ATPLUS 245-LQ- (TH),ATPLUS UEP 100LQ (CQ), Greenwet 7600, hydroxyl polyethylene oxide block copolymer (Agrilan 788 or Ethylan NS-500LQ), mono-comb polymer (Agrilan 755), sodium salt of alkyl naphthalene sulfonic acid polycondensate + block copolymer (Morwet D500), one or more of Nongru T-20, Nongru 0201B, Nongru 0203B, Nongru 1601, sodium naphthalene sulfonate formaldehyde condensate and sodium salt of methyl naphthalene sulfonate formaldehyde condensate;
the wetting agent may be selected from: ether compounds (Emulsson AG ISD90), organosilicon (SP-408), fatty alcohol ester sulfonate and plant alkene polyphenol polyether modifier mixture (SP-3266); one or more of polyethers (Greenwet510, Greenwet710, Greenwet730, Greenwet780 and Greenwet7618), a mixture of alkyl naphthalene sulfonate and an anionic wetting agent (Morwet EFW), and a block copolymer (Atlox 4894, Atlox 4896 or Tensiofix D33);
the thickening agent may be selected from: one or more of xanthan gum, magnesium aluminum silicate and white carbon black;
the antifoaming agent may be selected from: one or more of polydimethylsiloxane (SAG1522, SAG1572) and organic silicon (BS-163);
the anti-freeze agent may be selected from: ethylene glycol and/or glycerol.
Preferably, the dispersant is sodium polyacrylate (SD-811), polycarboxylate (SD819, Emulson TRN14105, SP-2750, GY-D800, DURAMAXTMD-205), carboxylate (SD815, SK-25CH), carboxylic acid macromolecule copolymer (Atlox 4913), sulfonate (SK-20TX, SK-24R), aryl ether phosphate (SK-33SC), gemini amphiphilic surfactant compound (SP-SC29), complex auxiliary agent (FS981) of polyacrylate copolymer, special structure macromolecule surfactant (SP-27001), EO/PO block polyether (D800 or Atlas G5000), block copolymer (Tensiofix AMS303 or Tensiofix XA265), macromolecule surfactant with 'ABA' regular structure (SP-2836), TWEEN L-LQ- (AP)), TWEEN L1010-LQ- (AP), hydroxypolyethylene oxide block copolymer (Agrilan 788 or Ethyllan NS-500LQ), single comb polymer (Agrilan 755), single comb polymer (Sklalan) and/or double comb polymer (Sklan) of, Sodium salt + block copolymer of alkyl naphthalene sulfonic acid polycondensate (Morwet D500), Nongru T-20, Nongru 0201B, Nongru 0203B, Nongru 1601, naphthalene sulfonic acidOne or more of sodium formaldehyde condensate and sodium salt of methyl sodium naphthalene sulfonate formaldehyde condensate;
the wetting agent is one or more of fatty alcohol ester sulfonate, plant alkene polyphenol polyether modifier mixture (SP-3266), alkyl naphthalene sulfonate and anionic wetting agent mixture (Morwet EFW), block copolymer (Atlox 4894, Tensiofix D33) and polyether (Greenwet510 and Greenwet 780);
the thickener is one or more of xanthan gum, white carbon black and magnesium aluminum silicate;
the defoaming agent is polydimethylsiloxane (SAG1522, SAG1572) and/or organosilicon (BS-163);
the antifreezing agent is ethylene glycol and/or glycerol.
Further preferably, the dispersant is one or more of sodium polyacrylate (SD-811), polycarboxylate (Emulson TRN14105, SP-2750), carboxylic acid polymer copolymer (Atlox 4913), sulfonate (SK-20TX, SK-24R), aryl ether phosphate (SK-33SC), gemini amphiphilic surfactant compound (SP-SC29), complexing auxiliary agent (FS981) of polyacrylate copolymer, special structure polymer surfactant (SP-27001), EO/PO block polyether (D800 or Atlas G5000), (Agrilan 788 or Ethyllan NS-500LQ), mono-comb polymer (Agrilan 755), sodium salt of alkyl naphthalene sulfonic acid polycondensate + block copolymer (Morwet D500), Nongru 0201B, Nongru 0203B and Nongru 1601;
the wetting agent is a mixture of fatty alcohol ester sulfonate and plant alkene polyphenol polyether modifier (SP-3266) and/or polyethers (Greenwet510, Greenwet 780);
the thickener is one or more of xanthan gum, white carbon black and magnesium aluminum silicate;
the defoaming agent is polydimethylsiloxane (SAG1522, SAG1572) and/or organosilicon (BS-163);
the antifreezing agent is ethylene glycol and/or glycerol.
The acaricide water suspending agent related by the invention is prepared by a conventional method, and the preparation method comprises the following steps: adding one of ethacrylonitrile, spirodiclofen, etoxazole and pyridaben, a dispersant, a wetting agent, a thickening agent, a defoaming agent, an antifreezing agent and water into a mixing tank according to a required proportion, uniformly mixing, firstly carrying out coarse crushing by a high-speed shearing machine, then pumping into a sand mill for fine grinding, and filtering when the average particle size of 95% of materials reaches below 5 mu m, thus obtaining the acaricide water suspension agent product.
The acaricide water suspending agent can be diluted before use or directly sprayed by mixing with water, and can also be directly used.
The method for preventing and controlling the pest mites by the acaricide water suspending agent comprises the following steps: the aqueous suspension of acaricide of the present invention is applied to the mites or their growth medium. An effective amount of from 10 grams per hectare to 1000 grams per hectare is generally preferred.
The application of the suspending agent containing the pyrazotoconazole and the spirodiclofen in preventing and treating pest mites in agriculture, forestry or sanitation. The acaricide water suspending agent can be applied to the control of agricultural pest mites, forestry pest mites or non-therapeutic purpose sanitary pest mites, especially has excellent control effect on pest mites such as tetranychus cinnabarinus, nymphs and mite eggs, and is safe to crops.
The invention has the advantages that:
according to the action target and the application mode thereof, the suspending agent adopts an auxiliary agent system matched with specific active ingredients to improve the wetting, spreading, dispersing, retaining and penetrating properties of the active ingredients on the crop target. By adopting the auxiliary agent system, the surface tension of the diluent used for spraying the sample prepared by the auxiliary agent system is close to or slightly lower than the surface tension of a target; the prepared sample has narrow particle size distribution, fine particles, small change of particle size distribution after long-term storage, good long-term storage stability and high utilization rate of effective components, thereby achieving the purposes of obviously improving the acaricidal activity, reducing the use cost and protecting the ecological environment;
the assistant system can prevent dispersed pesticide particles from aggregating again during dispensing and storage, so that the pesticide particles keep good dispersibility, appearance stability and heat storage stability, and the crystal growth speed is greatly reduced. Meanwhile, the diluent of the product prepared by the aid system has higher spreadability and adhesiveness on a control target, so that the wetting, spreading, dispersing, detention and permeability of the liquid medicine can be obviously improved, the drift of the sprayed liquid medicine along with wind (airflow) is reduced, the spreading and adhesion of the liquid medicine on leaf surfaces are facilitated, the biological activity of the liquid medicine is improved, the using amount of active ingredients of the pesticide is greatly reduced, the compatibility of the pesticide with the environment is improved, the cost is reduced, the quality of a pesticide preparation is improved, and the purpose of protecting the ecological environment is achieved; more specifically, the acaricide water suspending agent has the following advantages: 1) the particle size is small, the distribution is narrow, and the storage stability is good; low surface tension, good dispersibility, good fluidity, high suspension rate, high biological activity, small dosage, rain wash resistance, low residue, low toxicity to human and livestock, etc.; 2) the flash point is high, the material is not flammable or explosive, and the storage and the use are safe; 2) less dust, less environmental pollution, convenient application and safety to producers, users and environment; 3) after being sprayed, the water suspending agent is distributed on the surfaces of crops as fine particles, and the pesticide liquid is good in spreading and adhesion on the leaf surfaces and good in acaricidal effect; 4) labor and time are saved, and the purpose of preventing and controlling pests can be achieved by a reasonable application mode and the lowest medication cost.
Detailed Description
As known to those skilled in the art, the biological activity of the compounded two effective components is not affected by the high content or high weight percentage of the main components in the compounding, but based on the co-toxicity coefficient of the compounded effective components, the higher the co-toxicity coefficient of the mixture ratio is, the higher the biological activity is. The technical solutions in the embodiments of the present invention are clearly and completely described below, but the present invention is by no means limited to these examples. The embodiments of the present invention, and all other embodiments obtained by a person of ordinary skill in the art without any inventive work, belong to the scope of protection of the present invention. The percentages and parts in the formula are by weight. Chlorpyrifos (98% content, produced by Shenyang Kechuang chemical Co., Ltd.) is added according to dosage after being folded, and other raw materials are all commercial products.
Formulation examples of formulations
Example 1, 30% Chlorobipyr spirodiclofen suspension
According to the formula requirement, 15 parts of ethacrylonitrile, 15 parts of spirodiclofen, 4 parts of Emulson TRN14105, 2 parts of Tensiofix D33, 2 parts of SK-24R, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.5 part of SAG1522 and 5 parts of ethylene glycol are added into a mixing tank to be complemented to 100 percent, and are sequentially added into a mixing tank to be mixed, and are subjected to coarse crushing and homogenization through high shear, and then are pumped into a sand mill to be subjected to fine grinding, the particle size of the sand-milled material is detected through a particle size distribution instrument, and after the particle size reaches the standard requirement, the mixture is filtered, so that the 30 percent ethacrylonitrile-spirodiclofen suspending agent (shown in Table 1) can.
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 7.5; the suspension rate is more than 97 percent; pourability: residue after pouring 1.9%, residue after washing 0.2%; permanent foaming (after 1 min) 15 mL; the low-temperature stability is qualified; the thermal storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 1.5 percent.
TABLE 1 sample particle size Change before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.77 1.08 1.39 1.69 1.79
After heat storage (54 +/-2 ℃/14d) 0.78 1.09 1.41 1.7 1.8
Example 2, 30% Chlorobipyr-spirodiclofen suspension
According to the formula requirements, 15 parts of pyrazotoconazole, 15 parts of spirodiclofen, 4 parts of Emulson TRN14105, 3 parts of SP-SC29 and 3 parts of DURAMAXTMD-205, 3 parts of Greenwet510, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.5 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.1 part of BS163, 5 parts of ethylene glycol and water are added to 100% to be mixed in a mixing tank, coarse crushing and homogenization are performed through high shear, then the mixture is pumped into a sand mill to be finely ground, the particle size of the sand-ground material is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, filtration is performed to obtain the 30% ethazoxynil-spirodiclofen suspending agent (see Table 2).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 7.7; the suspension rate is more than 97 percent; pourability: residue after pouring 2.1%, residue after washing 0.3%; permanent foaming (after 1 min) 12 mL; the low-temperature stability is qualified; the thermal storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 1.5 percent.
TABLE 2 particle size variation of the samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.72 1.01 1.26 1.47 1.53
After heat storage (54 +/-2 ℃/14d) 0.75 1.04 1.29 1.56 1.65
Example 3, 30% Chlorobipyr-spirodiclofen suspension
According to the formula requirement, 15 parts of ethacrylonitrile, 15 parts of spirodiclofen, 3 parts of Atlox 4913, 2 parts of Ethylan NS-500LQ, 5 parts of SK-33SC, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 5 parts of glycerol and water are added to 100% in sequence and mixed in a mixing tank, coarse crushing and homogenization are carried out through high shear, then the mixture is pumped into a sand mill for fine grinding, the particle size of the ground material is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, filtration is carried out to obtain the 30% ethacrylonitrile-spirodiclofen suspending agent (shown in Table 3).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 7.5; the suspension rate is more than 98 percent; pourability: residue after pouring 1.9%, residue after washing 0.2%; permanent foaming (after 1 min) 10 mL; the low-temperature stability is qualified; the thermal storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 1.5 percent.
TABLE 3 particle size variation of the samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.69 0.98 1.3 1.66 1.76
After heat storage (54 +/-2 ℃/14d) 0.78 1.15 1.6 2.08 2.22
Example 4, 40% Chlorobipyr-spirodiclofen suspension
According to the formula requirement, 20 parts of ethacrylonitrile, 20 parts of spirodiclofen, 4 parts of SP-2750, 3 parts of Atlox 4913, 2 parts of TWEEN L1505-LQ- (AP), 3 parts of FS981, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.1 part of BS163 and 5 parts of ethylene glycol are added into a mixing tank to be complemented to 100 percent, and then the mixture is sequentially added into a mixing tank to be mixed, and is subjected to coarse crushing and homogenization through high shear, and then is pumped into a sand mill to be finely ground, the particle size of the sand-ground material is detected through a particle size distribution instrument, and after the particle size reaches the standard requirement, the mixture is filtered, so that the 40 percent of ethacrylonitrile-spirodiclofen suspending agent (.
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 6.9, the suspension percentage is more than 95%, and the pourability is as follows: 2.1% of residue after pouring, 0.3% of residue after washing, 28mL of lasting foamability (after 1 min), low-temperature stability and qualification; the thermal storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 1.5 percent.
TABLE 4 particle size variation of the samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 1.05 1.64 2.26 2.93 3.12
After heat storage (54 +/-2 ℃/14d) 1.57 2.52 3.68 4.95 5.28
Example 5, 6% Chlorobipyr-spirodiclofen suspension
According to the formula requirement, 1 part of ethacrylonitrile, 5 parts of spirodiclofen, 5 parts of SD811, 5 parts of Greenwet510, 2 parts of SK-20TX, 3 parts of agricultural milk 1601, 4 parts of agricultural milk 0203B, 0.15 part of xanthan gum, 0.18 part of sodium benzoate, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.5 part of SAG1522 and 5 parts of propylene glycol are added into a mixing tank to be mixed in sequence, the mixture is subjected to high shear, coarse crushing and homogenization, and then pumped into a sand mill to be subjected to fine grinding, a particle size distribution instrument is used for detecting the particle size of the sand-milled material, and after the particle size meets the standard requirement, the mixture is filtered to obtain the 6% ethacrylonitrile-spirodiclofen suspending agent (see Table 5).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: pH 7.2, suspension rate greater than 96%, pourability: 1.9% of residue after pouring, 0.2% of residue after washing, 10mL of lasting foamability (after 1 min), low-temperature stability and qualification; the thermal storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 1.5 percent.
TABLE 5 particle size variation of the samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.77 1.11 1.52 1.99 2.13
After heat storage (54 +/-2 ℃/14d) 0.9 1.51 3.22 5.28 5.73
Example 6, 18% Chlorobipyr-spirodiclofen suspension
According to the formula requirement, 16 parts of ethaboxam, 2 parts of spirodiclofen, 4 parts of agricultural milk 0201B, 2 parts of SK-20TX, 4 parts of SK-25CH, 3 parts of agricultural milk 1601, 0.15 part of xanthan gum, 0.18 part of sodium benzoate, 0.5 part of white carbon black, 0.5 part of magnesium aluminum silicate and 5 parts of ethylene glycol are added to 100% of water and are sequentially added into a mixing tank for mixing, coarse crushing and homogenization are performed through high shear, then the mixture is pumped into a sand mill for fine grinding, the particle size of the ground material is detected through a particle size distribution instrument, and after the particle size reaches the standard requirement, the mixture is filtered, so that the 18% ethaboxam spirodiclofen suspending agent (shown in Table 6) is obtained.
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 6.8, the suspension rate is more than 96%, and the pourability is as follows: 2.2% of residue after pouring, 0.3% of residue after washing, 20mL of lasting foamability (after 1 min), low-temperature stability and qualification; the thermal storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 1.5 percent.
TABLE 6 particle size variation of the samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.83 1.25 1.73 2.18 2.3
After heat storage (54 +/-2 ℃/14d) 0.9 1.4 1.94 2.46 2.62
Example 7, 20% Chlorobipyr-spirodiclofen suspension
According to the formula requirement, 15 parts of ethaboxam, 5 parts of spirodiclofen, 5 parts of SP-2836, 1 part of D800, 3 parts of SK-20TX, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.5 part of white carbon black, 0.5 part of magnesium aluminum silicate, 0.6 part of SAGA1522 and 5 parts of ethylene glycol are added to 100% by weight of water and are sequentially added into a mixing tank for mixing, coarse crushing and homogenization are carried out through high shear, then the mixture is pumped into a sand mill for fine grinding, the particle size of the ground material is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, the 20% ethaboxam spirodiclofen suspending agent (shown in Table 7) can be obtained through filtration.
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 6.9, the suspension rate is more than 93%, and the pourability is as follows: 2.0% of residue after pouring, 0.3% of residue after washing, 15mL of lasting foamability (after 1 min), low-temperature stability and qualification; the thermal storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 1.5 percent.
TABLE 7 particle size variation of the samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.79 1.15 1.49 1.81 1.89
After heat storage (54 +/-2 ℃/14d) 0.86 1.3 1.74 2.14 2.24
EXAMPLE 830% Chlorobipyr-spirodiclofen suspension (CN 104663668B published examples)
According to the formula requirement, 15 parts of ethaboxam, 15 parts of spirodiclofen, 4 parts of dispersing agent SP-28F, 3 parts of wetting agent SP-SC 3266, 2 parts of agricultural emulsion T-20, 0.1 part of xanthan gum, 0.5 part of white carbon black, 5 parts of ethylene glycol and water are complemented to 100 percent, are sequentially added into a mixing tank for mixing, are subjected to coarse crushing and homogenization through high shear, and then are pumped into a sand mill for fine grinding, the particle size of the materials is detected through a particle size distribution instrument, and after the particle size reaches the standard requirement, the 30 percent of ethaboxam spirodiclofen suspending agent is obtained through filtration (see table 8).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: pH 7.1, suspension rate greater than 95%, pourability: 2.2% of residue after pouring, 0.2% of residue after washing, 25mL of lasting foamability (after 1 min), low-temperature stability and qualification; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 8 particle size variation of the samples before and after storage
Figure BDA0001768839060000071
Figure BDA0001768839060000081
The surface tension of each of the formulations of examples 1 to 8 was also measured, and the above formulations were diluted with purified water, and then the surface tension of the diluted solution was measured using a surface tension meter, and the measurement results were obtained (see table 9).
TABLE 9 results of surface tension measurement of samples
Figure BDA0001768839060000082
Example 9, 24% Chlorpyrifos-Chlorpyrifos suspension
According to the formula requirement, 16 parts of ethaboxonitrile, 8 parts of pyridaben, 4 parts of SP-27001, 3 parts of Atlas G5000, 5 parts of SP-3266, 3 parts of SP-SC29, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.5 part of white carbon black, 0.5 part of magnesium aluminum silicate, 0.8 part of SAG1522 and 5 parts of ethylene glycol are added into a mixing tank in sequence to be supplemented to 100 percent, the mixture is mixed, the mixture is subjected to high shear, coarse crushing and homogenization, then the mixture is pumped into a sand mill to be finely ground, the particle size of the sand milled material is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, the mixture is filtered to obtain the 24 percent ethaboxonitrile pyridaben suspending agent (shown in Table 10).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 7.2; the suspension rate is more than 95 percent; pourability: residue after pouring 1.8%, residue after washing 0.2%; permanent foaming (after 1 min) 20 mL; the low-temperature stability is qualified; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 10 sample particle size Change before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.84 1.31 2.02 2.81 3.01
After heat storage (54 +/-2 ℃/14d) 0.93 1.52 2.28 3.11 3.33
Example 10, 24% Chlorpyrifos-Chlorpyrifos suspension
According to the formula requirement, 16 parts of ethazoxazonitrile, 8 parts of pyridaben, 4 parts of SK-25CH, 3 parts of Atlox 4894, 3 parts of SP-SC29, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.8 part of SAG1522 and 5 parts of ethylene glycol are added into a mixing tank to be supplemented to 100% by water, and are sequentially added into a mixing tank to be mixed, firstly subjected to high-shear coarse crushing and homogenization, and then pumped into a sand mill to be finely ground, the particle size of the sand-ground material is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, the 24% ethazoxazonitrile-pyridaben suspending agent is obtained by filtering (see table 11).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 7.5; the suspension rate is more than 95 percent; pourability: residue after pouring 2.1%, residue after washing 0.3%; permanent foaming (after 1 min) 15 mL; the low-temperature stability is qualified; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 11 particle size variation of samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.98 1.6 2.33 3.12 3.33
After heat storage (54 +/-2 ℃/14d) 1.06 1.71 2.43 3.2 3.41
Example 11, 24% Chlorpyrifos-Chlorpyrifos suspension
According to the formula requirement, 16 parts of ethacrylonitrile, 8 parts of pyridaben, 2 parts of Agrilan 755, 4 parts of Morwet D500, 4 parts of Tensiofix XA265, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.8 part of SAG1522 and 5 parts of ethylene glycol are added into a mixing tank in sequence to be complemented to 100 percent, the materials are mixed, firstly subjected to high-shear coarse crushing and homogenization, and then pumped into a sand mill to be finely ground, the particle size of the sand milled materials is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, the 24 percent of ethacrylonitrile pyridaben suspending agent (shown in Table 12) is obtained by filtering.
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 7.3; the suspension rate is more than 95 percent; pourability: residue after pouring 2.2%, residue after washing 0.3%; permanent foaming (after 1 min) 18 mL; the low-temperature stability is qualified; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 12 particle size variation of samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.87 1.3 1.8 2.29 2.43
After heat storage (54 +/-2 ℃/14d) 1.1 1.68 2.28 2.94 3.13
Example 12, 21% Chlorpyrifos-Chlorpyrifos suspension
According to the formula requirement, 1 part of ethazoxynil, 20 parts of pyridaben, 4 parts of agricultural emulsion 0201B, 3 parts of TWEEN L1505-LQ- (AP), 2 parts of SP-2836, 5 parts of SD819, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate and 5 parts of glycerol are added into a mixing tank to be supplemented to 100 percent, the materials are sequentially added into the mixing tank to be mixed, the materials are subjected to coarse crushing and homogenization through high shear, then the materials are pumped into a sand mill to be finely ground, the particle size of the ground materials is detected through a particle size distribution instrument, and after the particle size reaches the standard requirement, the materials are filtered to obtain the 21 percent ethazoxynil-pyridaben suspending agent (see table 13).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 7.5; the suspension rate is more than 95 percent; pourability: residue after pouring 1.9%, residue after washing 0.2%; permanent foaming (after 1 min) 15 mL; the low-temperature stability is qualified; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 13 particle size variation of samples before and after storage
Figure BDA0001768839060000091
Figure BDA0001768839060000101
Example 13, 33% Chlorpyrifos-Chlorpyrifos suspension
According to the formula requirement, 3 parts of ethacrylonitrile, 30 parts of pyridaben, 3 parts of TENSILOFIX DB08, 3 parts of Agrilan 788, 5 parts of Greenwet780, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.1 part of BS163 and 5 parts of ethylene glycol are added into a mixing tank to be supplemented to 100% by water, the mixture is sequentially added into a mixing tank to be mixed, the mixture is subjected to high-shear coarse crushing and homogenization, and then the mixture is pumped into a sand mill to be finely ground, the particle size of the sand milled material is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, the mixture is filtered to obtain the 33% ethacrylonitrile-pyridaben suspending agent (see Table 14).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: pH 7.1, suspension rate greater than 95%, pourability: 2.3% of residue after pouring and 0.3% of residue after washing, and 25mL of lasting foamability (after 1 min), low-temperature stability and qualification; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 14 particle size variation of the samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.98 1.57 2.28 3.09 3.3
After heat storage (54 +/-2 ℃/14d) 0.98 1.57 2.27 3.07 3.29
Example 14, 18% Chlorpyrifos-Chlorpyrifos suspension
According to the formula requirement, 12 parts of ethazoxynil, 6 parts of pyridaben, 4 parts of agricultural milk 0201B, 2 parts of SK-20TX, 4 parts of SK-25CH, 3 parts of agricultural milk 1601, 5 parts of Morwet D500, 0.15 part of xanthan gum, 0.18 part of sodium benzoate, 0.5 part of white carbon black, 0.5 part of magnesium aluminum silicate, 0.3 part of SAG1572 and 5 parts of ethylene glycol are added into a mixing tank in sequence to be complemented to 100 percent, coarse crushing and homogenization are carried out through high shearing, then the mixture is pumped into a sand mill to be finely ground, the particle size of the material is detected through a particle size distribution instrument, and after the particle size reaches the standard requirement of sand grinding, filtering is carried out, so that the 18 percent ethazoxynil-pyridaben suspending agent is obtained (see Table 15).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: pH 7.2, suspension rate greater than 95%, pourability: 1.9% of residue after pouring, 0.2% of residue after washing, 20mL of lasting foamability (after 1 min), low-temperature stability and qualification; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 15 particle size variation of samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.81 1.24 1.93 2.76 2.97
After heat storage (54 +/-2 ℃/14d) 0.94 1.51 2.22 3.04 3.26
Example 15, 24% Chlorpyrifos-pyridaben suspension (CN 104663666B published examples)
According to the formula requirement, 16 parts of ethazoxynil, 8 parts of pyridaben, 2 parts of sodium salt of a methyl naphthalene sulfonate formaldehyde condensate, 4 parts of polycarboxylate dispersant GY-D800, 2 parts of agricultural milk 1601, 4 parts of agricultural milk 0201B, 0.1 part of xanthan gum, 0.3 part of white carbon black, 5 parts of ethylene glycol and water are added to 100% in sequence and mixed, the mixture is subjected to high shear, coarse crushing and homogenization, then the mixture is pumped into a sand mill for fine grinding, the particle size of the sand-ground material is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, the mixture is filtered to obtain the 24% ethazoxynil-pyridaben suspending agent (shown in table 16).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 7.5; the suspension rate is more than 95 percent; pourability: residue after pouring 2.1%, residue after washing 0.3%; permanent foaming (after 1 min) 15 mL; the low-temperature stability is qualified; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 16 particle size variation of the samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 3.11 5.95 8.59 11.37 12.14
After heat storage (54 +/-2 ℃/14d) 3.14 6.11 8.77 11.51 12.29
The surface tension of each of the formulations of examples 9 to 15 was also measured by diluting the above formulations with purified water and then measuring the surface tension of the diluted solution with a surface tension meter (see table 17).
TABLE 17 results of surface tension measurement of samples
Figure BDA0001768839060000111
Example 16, 21% Etoxazole Acanthonitrile Etoxazole suspension
According to the formula requirement, 14 parts of pyrazotocast ethyl, 7 parts of etoxazole, 4 parts of TENSILOXX DB08, 3 parts of Tensiofix XA265, 2 parts of SK-20TX, 3 parts of Nongru 0203B, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.5 part of white carbon black, 0.5 part of magnesium aluminum silicate, 1 part of SAGA1522 and 5 parts of ethylene glycol are added into a mixing tank in sequence to be complemented to 100 percent, and then the mixture is added into a mixing tank to be mixed, firstly subjected to high shearing, coarse crushing and homogenization, and then pumped into a sand mill to be subjected to fine grinding, a particle size distribution instrument is used for detecting the particle size of the material, and after the sand mill reaches the standard requirement, the filtration is carried out, so that the 21 percent pyrazotocast ethyl-etoxazole suspending agent (see Table 18) can.
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: the pH value is 7.3; the suspension rate is more than 95 percent; pourability: residue after pouring 2%, residue after washing 0.2%; permanent foaming (after 1 min) 18 mL; the low-temperature stability is qualified; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 18 particle size variation of samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.67 0.95 1.24 1.54 1.65
After heat storage (54 +/-2 ℃/14d) 0.78 1.16 1.64 2.19 2.34
Example 1721% Etoxazole Acanthonitrile Etoxazole suspension
According to the formula requirement, 14 parts of pyraclonil, 7 parts of etoxazole, 4 parts of SP-2836, 5 parts of TWEEN L1010-LQ- (AP) and 5 parts of DURAMAXTMD-205, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.5 part of white carbon black, 0.5 part of magnesium aluminum silicate, 1 part of SAGA1522, 5 parts of ethylene glycol and water are added to 100% in sequence, the mixture is added into a mixing tank for mixing, the coarse grinding and the homogenization are carried out through high shear, then the mixture is pumped into a sand mill for fine grinding, the particle size of the sand-ground material is detected by a particle size distribution instrument, and the 21% ethacrylonitrile-etoxazole suspending agent can be obtained through filtration after the particle size reaches the standard requirement (see Table 19).
The results of the technical index tests performed on the suspensions obtained in the above examples are: pH 7.1, suspension rate greater than 95%, pourability: 2.5% of residue after pouring, 0.3% of residue after washing, 20mL of lasting foamability (after 1 min), low-temperature stability and qualification; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 19 particle size variation of samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.68 0.97 1.27 1.63 1.73
After heat storage (54 +/-2 ℃/14d) 0.89 1.43 2.05 2.68 2.86
Example 1821% Etoxazole mite nitrile Etoxazole suspension
According to the formula requirement, 14 parts of pyraclonil, 7 parts of etoxazole, 4 parts of D800, 3 parts of TANEMULL DA2880, 3 parts of Atlas G5000, 5 parts of Greenwet780, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.7 part of white carbon black, 0.7 part of magnesium aluminum silicate, 1 part of SAGA1522 and 5 parts of ethylene glycol are added into a mixing tank to be mixed in sequence, the mixture is subjected to high shear, coarse crushing and homogenization, then the mixture is pumped into a sand mill to be finely ground, the particle size of the sand milled material is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, the mixture is filtered to obtain 21% pyraclonil-etoxazole suspending agent (see table 20).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: pH 7.6, suspension rate greater than 95%, pourability: 2.2% of residue after pouring, 0.3% of residue after washing, 18mL of lasting foamability (after 1 min), low-temperature stability and qualification; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 20 particle size variation of samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.81 1.2 1.69 2.21 2.36
After heat storage (54 +/-2 ℃/14d) 0.87 1.35 1.87 2.43 2.58
Example 1936% Etoxazole mite nitrile Etoxazole suspension
According to the formula requirement, 30 parts of pyraclonil, 6 parts of etoxazole, 4 parts of TENSILOXIX DB08, 2 parts of Tensiofix AMS303, 2 parts of SP-2750, 5 parts of TANEMULL DA2880, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.5 part of white carbon black, 0.8 part of magnesium aluminum silicate and 5 parts of ethylene glycol are added into a mixing tank to be mixed, the mixture is added into a sand mill to be mixed in sequence, the mixture is subjected to high shear, coarse crushing and homogenization are performed, then the mixture is pumped into a sand mill to be finely ground, the particle size of the sand milled material is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, the mixture is filtered, so that 36% pyraclonil etoxazole suspending agent (see table 21) can be obtained.
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: pH 7.5, suspension rate greater than 95%, pourability: 1.9% of residue after pouring, 0.2% of residue after washing, 30mL of lasting foamability (after 1 min), low-temperature stability and qualification; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 21 particle size variation of samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.83 1.14 1.82 2.41 2.58
After heat storage (54 +/-2 ℃/14d) 0.92 1.26 1.82 2.7 2.94
Example 2021% Etoxazole Acanthonitrile Etoxazole suspension
According to the formula requirement, 20 parts of ethacrylonitrile, 1 part of etoxazole, 4 parts of a dispersing agent FS981, 1 part of a wetting agent SP-3266, 3 parts of Atlox 4913, 3 parts of SK-20TX, 2 parts of Tensiofix XA265, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.5 part of white carbon black and 5 parts of ethylene glycol are added into a mixing tank to be complemented to 100 percent, and are sequentially added into a sand mill to be mixed, and the mixture is subjected to high shearing, coarse grinding and homogenization, then is pumped into a sand mill to be finely ground, the particle size of the materials is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, the mixture is filtered to obtain the 21 percent of the ethacrylonitrile-etoxazole suspending agent (see table 22).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: pH 7.2, suspension rate greater than 95%, pourability: 1.8% of residue after pouring and 0.2% of residue after washing, and 15mL of lasting foamability (after 1 min), low-temperature stability and qualification; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 22 particle size variation of samples before and after storage
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 0.91 1.45 2.03 2.65 2.82
After heat storage (54 +/-2 ℃/14d) 0.93 1.46 2.04 2.65 2.83
Example 2121% Etoxazole mite nitrile Etoxazole suspension (CN 104663672B published examples)
According to the formula requirement, 14 parts of ethacrylonitrile, 7 parts of etoxazole, 2 parts of sodium naphthalene sulfonate formaldehyde condensate, 1 part of Morwet EFW, 2 parts of Nongru T-20, 4 parts of Nongru 0203B, 0.1 part of xanthan gum, 0.3 part of white carbon black, 5 parts of ethylene glycol and water are added to 100% in sequence and mixed, firstly, the mixture is subjected to high shear, coarse crushing and homogenization, then the mixture is pumped into a sand mill for fine grinding, the particle size of the materials is detected by a particle size distribution instrument, and after the particle size reaches the standard requirement, the mixture is filtered to obtain 21% of ethacrylonitrile-etoxazole suspending agent (see table 23).
The results of the technical index detection of the suspension obtained in the above embodiment are as follows: pH 7.5, suspension rate greater than 95%, pourability: 2.7% of residue after pouring, 0.3% of residue after washing, 18mL of lasting foamability (after 1 min), low-temperature stability and qualification; the heat storage stability (54 +/-2) DEG C/14 days, and the decomposition rate is less than 2 percent.
TABLE 23 particle size Change before and after storage of the samples
D50(μm) D75(μm) D90(μm) D97(μm) D98(μm)
Before storage 1.38 2.98 6.94 10.9 11.86
After heat storage (54 +/-2 ℃/14d) 1.48 3.16 7.08 9.71 10.36
The surface tension of each of the formulations of examples 16 to 21 was also measured by diluting the above formulations with purified water and then measuring the surface tension of the diluted solutions with a surface tension meter (see Table 24).
TABLE 24 results of surface tension measurement of samples
Figure BDA0001768839060000141
The sample prepared by the specific auxiliary agent system has narrow particle size distribution, fine particles, small change of particle size distribution after long-term storage, good long-term storage stability and high utilization rate of effective components, and the auxiliary agent system can prevent dispersed pesticide particles from aggregating again during dispensing and storage, so that the dispersed pesticide particles keep good dispersibility, appearance stability and heat storage stability, and the crystal growth speed is greatly reduced. Meanwhile, the diluent of the product prepared by the aid system has higher spreadability and adhesiveness on a control target (for controlling agricultural, forestry or sanitary pest mites), so that the wetting, spreading, dispersing, detenting and penetrating properties of the liquid medicine can be obviously improved, the drift of the sprayed liquid medicine along with wind (airflow) is reduced, and further, the suspending agent has small particle size, narrow distribution and good storage stability; low surface tension, good dispersibility, good fluidity, high suspension rate, high bioactivity, small dosage, rain wash resistance, low residue, low toxicity to human and livestock, etc.
Examples of biological Activity test
Example 22 comparative test for biological Activity
The test method comprises the following steps: the activity of different batches of test samples on tetranychus cinnabarinus adults is determined by a potted seedling spraying method. Firstly, inoculating tetranychus cinnabarinus with consistent size to kidney bean seedling leaves in a first true leaf flattening period, and counting the base number after the tetranychus cinnabarinus is stabilized; then evenly spraying 2mL of each plant from low dose to high dose according to the experimental design, repeating each treatment for 3 times, and setting a blank control. The treated test specimen was placed in an observation room under certain conditions, the number of dead and alive mites was periodically investigated, and the mortality was calculated as shown in tables 25 to 27 (mortality was calculated by Abbot formula, LC was calculated by DPS software)50Values and 95% confidence limits).
TABLE 25 indoor bioactivity assay results of E-Metronidazole and spirodiclofen suspension samples on Tetranychus cinnabarinus
Figure BDA0001768839060000142
Figure BDA0001768839060000151
TABLE 26 indoor bioactivity assay results for Metronidazole and pyridaben suspension samples on Tetranychus cinnabarinus
Figure BDA0001768839060000152
TABLE 27 indoor bioactivity determination results of E-Metronidazole and E-Metronidazole suspension samples on Tetranychus cinnabarinus
Figure BDA0001768839060000153
The above experimental results show that the biological activities of the samples prepared in examples 1 to 3, 9 to 11, and 16 to 18 of the present invention are significantly different from those of the corresponding technical material and the samples prepared in the prior art (example 8, example 15, and example 21). Namely, under the same dosage, the acaricide has obvious synergy to tetranychus cinnabarinus, is an ideal acaricide variety, and accords with the national pesticide application reduction and synergy policy.
The water suspending agent has good compatibility to the environment, does not increase the toxicity of the raw pesticide to mammals, and does not generate phytotoxicity to crops; the pesticide has good chemical stability to the original pesticide; the biological activity of the effective ingredients of the pesticide is not reduced; during the use process, the dispersion degree of the effective components and the deposition amount and the deposition proportion of the effective components to the target body can be improved; indoor biological activity determination shows that the composition suspending agent has obvious synergy, small using amount and strong strain capacity to use technical conditions.

Claims (2)

1. A suspending agent containing a pyraclonil composition is characterized in that:
the 24% ethiprole pyridaben suspending agent is 16 parts of ethiprole, 8 parts of pyridaben, 4 parts of SP-27001, 3 parts of Atlas G5000, 5 parts of SP-3266, 3 parts of SP-SC29, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.5 part of white carbon black, 0.5 part of magnesium aluminum silicate, 0.8 part of SAG1522, 5 parts of glycol and water for supplementing to 100%;
or 16 parts of ethacrylonitrile, 8 parts of pyridaben, 4 parts of SK-25CH, 3 parts of Atlox 4894, 3 parts of SP-SC29, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.8 part of SAG1522, 5 parts of ethylene glycol and the balance of water to 100 percent;
or 16 parts of ethacrylonitrile, 8 parts of pyridaben, 2 parts of Agrilan 755, 4 parts of Morwet D500, 4 parts of Tensiofix XA265, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.8 part of SAG1522, 5 parts of ethylene glycol and water to make up to 100 percent;
or the 30% ethacrylonitrile spirodiclofen suspending agent is 15 parts of ethacrylonitrile, 15 parts of spirodiclofen, 4 parts of Emulson TRN14105, 2 parts of Tensiofix D33, 2 parts of SK-24R, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.5 part of SAG1522, 5 parts of ethylene glycol and water for supplementing to 100%;
or 15 parts of pyrazotoconazole, 15 parts of spirodiclofen, 4 parts of Emulson TRN14105, 3 parts of SP-SC29, 3 parts of DURAMAXTMD-205, 3 parts of Greenwet510, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.5 part of white carbon black, 0.8 part of magnesium aluminum silicate, 0.1 part of BS163, 5 parts of ethylene glycol and water to make up to 100 percent;
or 15 parts of ethacrylonitrile, 15 parts of spirodiclofen, 3 parts of Atlox 4913, 2 parts of Ethylan NS-500LQ, 5 parts of SK-33SC, 0.1 part of xanthan gum, 0.12 part of sodium benzoate, 0.8 part of white carbon black, 0.8 part of magnesium aluminum silicate, 5 parts of glycerol and water for supplementing to 100 percent;
or the 21% ethiprole and etoxazole suspending agent is 14 parts of ethiprole, 7 parts of etoxazole, 4 parts of TENSIOFIX DB08, 3 parts of Tensiofix XA265, 2 parts of SK-20TX, 3 parts of Nongru 0203B, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.5 part of white carbon black, 0.5 part of magnesium aluminum silicate, 1 part of SAGA1522, 5 parts of glycol and water to make up to 100%;
or 14 parts of pyrazotoconazole, 7 parts of etoxazole, 4 parts of SP-2836, 5 parts of TWEEN L1010-LQ- (AP) and 5 parts of DURAMAXTMD-205, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.5 part of white carbon black, 0.5 part of magnesium aluminum silicate, 1 part of SAGA1522, 5 parts of ethylene glycol and water to make up to 100 percent;
or 14 parts of pyrazoxynil, 7 parts of etoxazole, 4 parts of D800, 3 parts of TANEMULL DA2880, 3 parts of Atlas G5000, 5 parts of Greenwet780, 0.1 part of xanthan gum, 0.12 part of BITEBAN GIOS, 0.7 part of white carbon black, 0.7 part of magnesium aluminum silicate, 1 part of SAGA1522, 5 parts of ethylene glycol and water to make up to 100 percent;
the percentages and parts in the formula are by weight.
2. The use of the suspension concentrate containing ethacrylonitrile and spirodiclofen according to claim 1 for controlling harmful mites in agriculture, forestry or hygiene.
CN201810940138.8A 2018-08-17 2018-08-17 Suspending agent containing pyraclostrobin composition and application thereof Active CN108902158B (en)

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CN111149799A (en) * 2020-02-19 2020-05-15 中国日用化学研究院有限公司 Multifunctional pesticide aqueous suspension dispersant, preparation method and use method thereof
CN111990398A (en) * 2020-07-27 2020-11-27 南京太化化工有限公司 Auxiliary agent for suspending agent and cyromazine suspending agent
CN112155012A (en) * 2020-10-14 2021-01-01 天津市汉邦植物保护剂有限责任公司 Water suspending agent containing ivermectin and chlorfenapyr and preparation method and application thereof
CN114642210B (en) * 2021-04-06 2024-05-28 山东统防生物科技有限公司 Suspending agent containing methoxy carbamate and cyazofamid and application thereof
CN114642211B (en) * 2021-04-06 2024-05-28 山东统防生物科技有限公司 Chlorantraniliprole and chlorfenapyr composition and preparation method thereof
CN114431248B (en) * 2022-02-07 2023-09-01 陕西先农生物科技有限公司 Suspending agent containing avermectin and chlorantraniliprole

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