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CN108902156B - Composite bactericidal suspending agent and preparation method thereof - Google Patents

Composite bactericidal suspending agent and preparation method thereof Download PDF

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Publication number
CN108902156B
CN108902156B CN201810559733.7A CN201810559733A CN108902156B CN 108902156 B CN108902156 B CN 108902156B CN 201810559733 A CN201810559733 A CN 201810559733A CN 108902156 B CN108902156 B CN 108902156B
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suspending agent
parts
chlorothalonil
azoxystrobin
agent
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CN108902156A (en
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王娅婷
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Pilarquim Shanghai Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/541,3-Diazines; Hydrogenated 1,3-diazines
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/34Nitriles

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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 relates to a composite bactericidal suspending agent and a preparation method thereof, belongs to the technical field of pesticides, and aims to solve the problem of poor stability of a suspending agent compounded by azoxystrobin and chlorothalonil. The technical scheme is as follows: the composite bactericidal suspending agent consists of the following components in parts by weight: 3-12 parts of azoxystrobin, 35-55 parts of chlorothalonil, 3-10 parts of a surfactant, 0.04-0.16 part of a thickening agent, 2-8 parts of an antifreeze agent, 0.1-1 part of a synergist and 35-45 parts of soft water. The invention has the effect of good stability of the suspending agent in the storage process, and is used for preventing and controlling diseases of various crops.

Description

Composite bactericidal suspending agent and preparation method thereof
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to a composite bactericidal suspending agent and a preparation method thereof.
Background
The suspending agent is a preparation which is prepared by uniformly dispersing the original pesticide in water in a particle form and has the advantages of no dust hazard, small particles, large active surface and strong permeability. However, the suspending agent is a thermodynamically unstable system, and during the storage period of the suspending agent, the state of the suspending agent is easy to change, and quality problems such as reduction of the suspension rate, delamination, bottom formation and the like occur. In combination with stokes' law, the physical storage stability of a suspending agent is related to the particle size of suspended particles in the formulation, the viscosity of the formulation and the density difference. The particle size and the particle spectrum distribution of the suspension particles of the preparation are influenced by various factors, such as the self property of the pesticide active ingredient, the types and the dosage of the auxiliary agents, the processing conditions and the like.
In the prior art, Chinese patent with publication number CN100376157C discloses a bactericidal composition containing azoxystrobin and chlorothalonil and application thereof, wherein the bactericidal composition containing azoxystrobin and chlorothalonil is a suspending agent, and sodium dodecyl sulfate, nonylphenol polyoxyethylene ether, a dispersing agent NNO, xanthan gum and the like are adopted as auxiliaries to prepare the water suspending agent containing azoxystrobin and chlorothalonil. The suspension concentrates prepared according to the above-mentioned methods still have the problem of poor physical stability during storage.
Disclosure of Invention
The invention aims to provide a composite bactericidal suspending agent and a preparation method thereof, and the composite bactericidal suspending agent has the advantage of good stability.
The technical purpose of the invention is realized by the following technical scheme: the composite bactericidal suspending agent consists of the following components in parts by weight: 3-12 parts of azoxystrobin, 35-55 parts of chlorothalonil, 3-10 parts of a surfactant, 0.04-0.16 part of a thickening agent, 2-8 parts of an antifreeze agent, 0.1-1 part of a synergist and 35-45 parts of soft water.
By implementing the technical scheme, the surfactant is beneficial to improving the dispersing performance of the azoxystrobin and the chlorothalonil, reduces the sedimentation and agglomeration of the particles, promotes the uniform dispersion of the azoxystrobin and the chlorothalonil particles in water, and has the function of keeping a relatively stable dispersion system. The thickening agent is a rheological additive, so that the rheological property of the suspending agent can be adjusted, solid particles can be supported, and the azoxystrobin and the chlorothalonil have good suspending capability. The antifreeze agent is beneficial to improving the storage stability of the suspending agent in a low-temperature environment, and the synergist is beneficial to enhancing the adhesion of the azoxystrobin and the chlorothalonil on target crops and prolonging the action time of the bactericidal suspending agent. The surfactant, the thickening agent and the anti-freezing agent are matched to improve the stability of the suspending agent of the product.
Further, the paint comprises the following components in parts by weight: 5-10 parts of azoxystrobin, 38-45 parts of chlorothalonil, 5-8 parts of a surfactant, 0.06-0.1 part of a thickening agent, 3-5 parts of an antifreeze agent, 0.1-0.3 part of a synergist and 38-42 parts of soft water.
By implementing the technical scheme, the proportion of the components is favorable for the storage stability of the sterilizing suspending agent.
Further, the surfactant is one or more of phosphate, alkyl sulfonate and polycarboxylic acid.
By implementing the technical scheme, the phosphate, alkyl sulfonate and polycarboxylic acid surfactant belong to anionic surfactants, and the phosphate, alkyl sulfonate and polycarboxylic acid surfactant have uniform and good dispersion effects, so that solid particles are uniformly dispersed in water.
Further, the surfactant comprises 2-5 parts by weight of phosphate, 1-3 parts by weight of carboxylate and 0.1-1 part by weight of alkyl sulfonate.
Further, the surfactant comprises 3-4.5 parts by weight of phosphate, 1.5-2.2 parts by weight of carboxylate and 0.3-0.6 part by weight of alkyl sulfonate.
By implementing the technical scheme, the phosphate ester, alkyl sulfonate and carboxylate surfactants are compounded according to the proportion, and in a suspension system formed by the surfactants, the azoxystrobin and chlorothalonil can maintain the smaller (less than 3 mu m) particle size of particles, so that the stability of the azoxystrobin and chlorothalonil is favorably maintained, the storage stability of the bactericidal suspension agent is favorably improved, and the stable exertion of the pesticide effect is further favorably realized.
Further, the thickener is xanthan gum.
By implementing the technical scheme, the xanthan gum enhances the stability of the system by improving the viscosity of the system. The xanthan gum can form a banded spiral copolymer to form a mesh structure similar to gum, and is favorable for supporting the suspension effect of azoxystrobin and chlorothalonil solid particles.
Further, the antifreeze is one or more of ethylene glycol, propylene glycol and glycerol.
By implementing the technical scheme, the antifreeze can reduce the freezing point of water and improve the antifreeze capacity of the suspending agent. The ethylene glycol is mixed with water to lower the freezing point of the water by changing the vapor pressure of the water, so that the suspending agent can keep a stable system when stored at low temperature.
Further, the synergist is ADJ-81N.
By implementing the technical scheme, the ADJ-81N is an auxiliary agent purchased from Japanese bamboo oil, has a chemical name of ethoxy resin, has a developed bonding effect, is beneficial to the adhesion of azoxystrobin and chlorothalonil on target crops, and further achieves the effects of prolonging the pesticide effect period and enhancing the pesticide effect.
The invention also aims to provide a preparation method of the composite sterilizing suspending agent, which is characterized by comprising the following steps:
step one, dissolving a thickening agent into 1-2% aqueous solution by mass percent with soft water, and placing the aqueous solution in a shearing machine for shearing for 20-40 min to obtain a thickened solution for later use.
And step two, sequentially adding the rest soft water, the azoxystrobin, the chlorothalonil, the surfactant and the antifreeze into a stirrer, and uniformly mixing to obtain a mixed solution.
And step three, grinding the mixed solution obtained in the step one in a sand grinder, and grinding the particles in the mixed solution to 2-3 microns to obtain the grinding fluid.
And step four, adding the thickening solution and the synergist into the grinding liquid, and uniformly stirring to obtain the bactericidal suspending agent.
By implementing the technical scheme, the viscosity of the xanthan gum aqueous solution is not easy to disperse in the suspension because the viscosity of the xanthan gum aqueous solution is high, the viscosity of the xanthan gum aqueous solution is required to be reduced by processing with a shearing machine to be fully mixed with the mixed solution, and after the shearing action is removed, the viscosity of the xanthan gum in water is recovered, so that the viscosity of the suspension system is improved, and a supporting effect is formed on solid particles in the suspension.
Further, the grinding time in the third step is 75-100 min.
In conclusion, the invention has the following beneficial effects:
by compounding the azoxystrobin and the chlorothalonil with the surfactant, the thickening agent and the antifreeze agent according to a fixed proportion, the bactericidal suspending agent compounded by the azoxystrobin and the chlorothalonil has good stability and dispersibility, which is beneficial to maintaining the particle size of less than three microns and a uniform dispersion state of the azoxystrobin and chlorothalonil particles in the suspending agent in the storage process, thereby promoting the suspending agent to stably exert the drug effect. The addition of the synergist is beneficial to enhancing the adhesion of the drug effect components on target crops, so that the drug effect components are not easily washed away by rainwater, and the effects of prolonging the drug effect period and enhancing the drug effect are achieved.
Detailed Description
The present invention will be described in further detail with reference to examples.
The first embodiment is as follows:
the embodiment relates to a composite bactericidal suspending agent which is prepared from the following raw materials: 1.5kg azoxystrobin, 17.5kg chlorothalonil, 1kg YUS-FS3000, 0.5kg PICO-CH7000, 0.05kg YUS-SXC, 0.04kg xanthan gum, 1kg propylene glycol, 0.05kg ADJ-81N and 17.5kg soft water. The auxiliaries used in this example and in the following examples, YUS-FS3000, PICO-CH7000 and YUS-SXC, were obtained from Japanese bamboo fat.
The composite bactericidal suspending agent is prepared by the following method:
step one, dissolving xanthan gum into an aqueous solution with the mass percent of 2% by using soft water, namely dissolving 0.04kg of xanthan gum by using 2kg of soft water, and placing the aqueous solution in a shearing machine for shearing for 20min to obtain a thickened solution for later use.
And step two, sequentially adding the rest soft water, namely 15.5kg of soft water, azoxystrobin, chlorothalonil, YUS-FS3000, PICO-CH7000, YUS-SXC and propylene glycol into a stirrer, and uniformly mixing to obtain a mixed solution.
And step three, grinding the mixed solution obtained in the step one in a sand grinder for 75min, and grinding the particles in the mixed solution to 2 microns to obtain the grinding fluid.
And step four, adding the thickening solution and ADJ-81N into the grinding liquid, and uniformly stirring to obtain the bactericidal suspending agent.
Example two:
the embodiment relates to a composite bactericidal suspending agent which is prepared from the following raw materials: 4kg of azoxystrobin, 30.4kg of chlorothalonil, 2.4kg of YUS-FS3000, 1.2kg of PICO-CH7000, 0.24kg of YUS-SXC, 0.048kg of xanthan gum, 2.4kg of glycerol, 0.24kg of ADJ-81N and 30.4kg of soft water.
The composite bactericidal suspending agent is prepared by the following method:
step one, dissolving polyvinyl alcohol into 1% water solution by mass percent by using soft water, namely dissolving 0.048kg of xanthan gum by using 4.8kg of soft water, and placing the water solution in a shearing machine for shearing for 30min to obtain a thickened solution for later use.
And step two, sequentially adding the rest soft water, namely 25.6kg of soft water, azoxystrobin, chlorothalonil, YUS-FS3000, PICO-CH7000, YUS-SXC and glycerol into a stirrer, and uniformly mixing to obtain a mixed solution.
And step three, grinding the mixed solution obtained in the step one in a sand mill for 90min, and grinding the particles in the mixed solution to 2.5 microns to obtain the grinding fluid.
And step four, adding the thickening solution and ADJ-81N into the grinding liquid, and uniformly stirring to obtain the bactericidal suspending agent.
Example three:
the embodiment relates to a composite bactericidal suspending agent which is prepared from the following raw materials: 4.1kg azoxystrobin, 20.5kg chlorothalonil, 2kg YUS-FS3000, 1kg PICO-CH7000, 0.25kg YUS-SXC, 0.08kg xanthan gum, 2kg ethylene glycol, 0.25kg ADJ-81N and 20.1kg soft water.
The composite bactericidal suspending agent is prepared by the following method:
step one, dissolving polyvinyl alcohol into an aqueous solution with the mass percent of 2% by using soft water, namely dissolving 0.08kg of xanthan gum by using 4kg of soft water, and placing the aqueous solution in a shearing machine for shearing for 40min to obtain a thickened solution for later use.
And step two, sequentially adding the rest soft water, namely 16.1kg of soft water, azoxystrobin, chlorothalonil, YUS-FS3000, PICO-CH7000, YUS-SXC and ethylene glycol into a stirrer, and uniformly mixing to obtain a mixed solution.
And step three, grinding the mixed solution obtained in the step one in a grinder for 100min, and grinding the particles in the mixed solution to 3 microns to obtain the grinding fluid.
And step four, adding the thickening solution and ADJ-81N into the grinding liquid, and uniformly stirring to obtain the bactericidal suspending agent.
Examples four to seven:
the preparation method of the composite bactericidal suspending agent is the same as the two examples, and the specific compositions and the using amounts of the examples are shown in table 1.
Table 1 ingredients and amounts used in the examples
Composition (I) Example one Example two EXAMPLE III Example four EXAMPLE five EXAMPLE six EXAMPLE seven
Azoxystrobin 1.5 4 4.1 5 7.2 3.2 4.8
Chlorothalonil 17.5 30.4 20.5 22.5 33 16 24
YUS-FS3000 1 2.4 2 2.25 3 1.2 0
PICO-CH7000 0.5 1.2 1 1.1 1.8 0 0
YUS-SXC 0.05 0.24 0.25 0.3 0.6 0 6
Xanthan gum 0.04 0.048 0.08 0.05 0.096 0.032 0.048
Ethylene glycol 0 0 2 2.5 0 0 0
Propylene glycol 1 0 0 0 2.4 1.6 0
Glycerol 0 2.4 0 0 2.4 0 2.4
ADJ-81N 0.05 0.24 0.25 0.5 0.18 0.24 0.24
Soft water 17.5 30.4 20.1 21 27 16 24
The dosage units of the components in table 1 are in kg.
Comparative example one:
the difference between the comparative example and the second embodiment is mainly as follows: the composite bactericidal suspending agent does not contain a thickening agent.
Comparative example two:
10kg of azoxystrobin, 14kg of chlorothalonil, 3kg of sodium dodecyl sulfate, 2kg of nonylphenol polyoxyethylene ether, 2kg of expand stand alone NNO, 0.15kg of xanthan gum, 5kg of propylene glycol and 20kg of water are mixed, and the mixture is ground and homogenized by a wet method to prepare the aqueous suspension.
Product detection
The low temperature stability of the products of each example and comparative example was tested according to GB/T19137-2003 and the results of sieve analysis and suspension rate measurements are shown in Table 2.
The respective examples and comparative products were stored at room temperature for three months, and then the particle size distribution in each product was measured by a laser particle size distribution meter, and the measurement results are shown in Table 2.
TABLE 2 examination results of examples and comparative examples
Figure BDA0001683009870000051
As can be seen from table 2, the suspension concentrate compositions prepared according to the first to seventh embodiments have good low-temperature stability, and the product prepared according to the first comparative example does not meet the national standards in terms of low-temperature stability. The particle size distribution measurement results of products prepared in each example and comparative example after being stored for three months show that the technical schemes in the first to fifth examples have excellent stability, the particle size of particles in the suspending agent is basically maintained at a level of less than 5 micrometers, and the particle size of particles in the third and fourth examples is basically maintained at a level of 2-3 micrometers. In the suspending agents prepared in the first and second comparative examples, the particle diameters of azoxystrobin and chlorothalonil are obviously more than 5 microns, and the compound proportion of azoxystrobin and chlorothalonil and the suspending agent prepared by compounding the azoxystrobin and chlorothalonil with other auxiliary agents are proved to have poor stability. Compared with the measurement results of two comparative products, the suspending agent prepared according to the technical scheme of the invention has good stability, is beneficial to improving the storage stability of the sterilizing suspending agent, and is further beneficial to the stable exertion of the drug effect.
The above examples are only used to illustrate the technical solutions of the present invention, and do not limit the scope of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from these embodiments without making any inventive step, fall within the scope of the present invention.

Claims (2)

1. The composite bactericidal suspending agent is characterized by comprising the following components in parts by mass: 3.2kg of azoxystrobin, 16kg of chlorothalonil, YUS-FS30001.2kg, 0.032kg of xanthan gum, 1.6kg of propylene glycol, 0.24kg of ADJ-81N and 16kg of soft water.
2. The composite bactericidal suspending agent is characterized by comprising the following components in parts by mass: 4.8kg of azoxystrobin, 24kg of chlorothalonil, 6kg of YUS-SXC, 0.048kg of xanthan gum, 2.4kg of glycerol, 0.24kg of ADJ-81N and 24kg of soft water.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105085049A (en) * 2015-08-17 2015-11-25 北京沃土天地生物科技有限公司 High-nitrogen suspension-type liquid fertilizer and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB0021786D0 (en) * 2000-09-05 2000-10-18 Zeneca Ltd Fungicidal formulations
CN100376157C (en) * 2005-09-15 2008-03-26 南京第一农药有限公司 Germicide composition containing kresoxim-methyl and chlorothalonil and its application
CN102057912B (en) * 2010-12-19 2013-04-17 惠州市银农科技有限公司 Water suspending agent mixed by difenoconazole and azoxystrobin and preparation method thereof
CN102669111B (en) * 2012-05-24 2014-06-04 利民化工股份有限公司 Suspending agent formulated by difenoconazole and azoxystrobin and preparation method thereof
CN102726403A (en) * 2012-06-09 2012-10-17 广东中迅农科股份有限公司 Azoxystrobin suspension concentrate and preparation method thereof

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105085049A (en) * 2015-08-17 2015-11-25 北京沃土天地生物科技有限公司 High-nitrogen suspension-type liquid fertilizer and preparation method thereof

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