CN115812721A - Spinosad suspending agent and preparation method and application thereof - Google Patents

Spinosad suspending agent and preparation method and application thereof Download PDF

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Publication number
CN115812721A
CN115812721A CN202210010159.6A CN202210010159A CN115812721A CN 115812721 A CN115812721 A CN 115812721A CN 202210010159 A CN202210010159 A CN 202210010159A CN 115812721 A CN115812721 A CN 115812721A
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spinosad
spinosyn
suspension
agent
suspending agent
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余徳勉
王陈杰
万娜娜
张常庆
侯影
宋怀挺
魏宁
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Shanghai Yuelian Biotechnology Co ltd
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Shanghai Yuelian Biotechnology Co ltd
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    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract

The invention relates to the technical field of A01N25/04, and particularly relates to a spinosad suspending agent, and a preparation method and application thereof. A preparation raw material of a spinosad suspending agent comprises spinosad and a component B, wherein the component B is selected from one or more of chlorantraniliprole, indoxacarb and methoxyfenozide. The spinosad suspending agent prepared by compounding the spinosad, chlorantraniliprole, indoxacarb and methoxyfenozide has a good insecticidal effect, particularly has excellent insecticidal activity to agricultural lepidoptera pests such as cotton bollworm, plutella xylostella, cabbage caterpillar, beet armyworm, prodenia litura, cabbage prodenia plutella and the like, is particularly suitable for prodenia litura and cabbage prodenia litura, is beneficial to delaying the generation of insect resistance, can prolong the service life of pesticide varieties, reduces the use dosage, reduces the pollution to the environment, and has a good application value in the aspects of treatment and comprehensive prevention of the drug resistance of prodenia litura and cabbage armyworm.

Description

Spinosad suspending agent and preparation method and application thereof
Technical Field
The invention relates to the technical field of A01N25/04, and particularly relates to a spinosad suspending agent, and a preparation method and application thereof.
Background
Chinese patent with patent application number CN201010216510.4 discloses an insecticidal composition containing methoxyfenozide and a biological source insecticide, which adopts methoxyfenozide and spinosad, solves the problem of better control of winged pests in crops, but does not disclose and solve the technical problems of reducing lasting foamability, quickly defoaming, avoiding pouring residues, improving sanding stability and improving grain size stability in the storage process.
Disclosure of Invention
In order to solve the problems, the invention provides a spinosad suspension, which is prepared from the raw materials of spinosad and a component B, wherein the component B is one or more selected from chlorantraniliprole, indoxacarb and methoxyfenozide.
Preferably, the preparation raw materials of the spinosad suspending agent comprise 8-15wt% of spinosad and the component B by weight percentage.
Preferably, the weight ratio of the spinosad to the chlorantraniliprole is (1-5): (1-5).
Preferably, the weight ratio of the spinosad to the indoxacarb is (1-3): (1-9).
Preferably, the weight ratio of the spinosad to the methoxyfenozide is (1-5): (1-5).
Spinosad is a macrolide nuisance-free high-efficiency biopesticide extracted from sugarcane polyspora spinosa fermentation liquor.
The chlorantraniliprole belongs to o-formylaminobenzoyl insecticides, can control lepidoptera pests of various crops, and has better control effect on other pests.
Indoxacarb belongs to a broad-spectrum oxadiazine pesticide, has the stomach poisoning contact effect, and can effectively prevent and control various pests.
Methoxyfenozide belongs to an insect growth regulator, can interfere the normal growth and development of insects, and has effects of stomach toxicity, and specific contact poisoning and ovicidal activity.
Provides high bactericidal effect, expands bactericidal spectrum and avoids pesticide residue and drug resistance. The inventor finds that the spinosad can be used for continuously activating the acetylcholine nicotinic receptor of the target insect by utilizing the special binding site thereof, can be combined with other components such as chlorantraniliprole/indoxacarb/methoxyfenozide and the like to promote the insecticidal effect, has no cross resistance, can expand the insecticidal spectrum and improve the application range.
Preferably, the preparation raw materials of the spinosad suspending agent comprise, by weight, 6-10wt% of a dispersing agent, 1-3wt% of a wetting agent, 0.5-1.5wt% of a thickening agent and the balance of water.
Preferably, the dispersing agent is selected from one or more of fatty alcohol-polyoxyethylene ether phosphate, calcium lignosulfonate, anionic polycarboxylate, sodium methylene-bis-naphthalene sulfonate, vinyl bis-stearamide and alkyl naphthalene sulfonate formaldehyde condensate.
Preferably, the dispersing agent comprises fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate and vinyl bis stearamide, and the weight ratio of the fatty alcohol-polyoxyethylene ether phosphate to the anionic polycarboxylate to the vinyl bis stearamide is (3-5): (2-4): 1.
the anionic polycarboxylate is a macromolecular compound with carboxyl, sulfonic group, amino and polyoxyethylene side chain, belongs to an anionic surfactant, does not contain harmful substances such as naphthalene, formaldehyde and the like, and reduces the pollution to the environment.
The anionic polycarboxylate was purchased from Hensman USA under the TER-SPERSE 2700 model.
In a preferred embodiment, as examples of the fatty alcohol polyoxyethylene ether phosphate, C12-18 fatty alcohol polyoxyethylene ether phosphate, such as AEO-3P, AEO-5P, AEO-7P, and AEO-9P, wherein the number following AEO indicates the degree of polymerization of EO, can be cited. Preferably, the EO degree of polymerization of the fatty alcohol-polyoxyethylene ether phosphate is 3-5.
In a preferable technical scheme, the fatty alcohol-polyoxyethylene ether phosphate is C12-14 fatty alcohol-polyoxyethylene ether phosphate,
the C12-14 fatty alcohol polyoxyethylene ether phosphate is purchased from chemical technology Co, ltd in North Hu east, and the model is AEO-3P.
The CAS number of the vinyl bis-stearamide is 110-30-5.
The inventor finds that the active ingredient outer micelle collision is increased with the increase of the storage time, particularly at higher temperature, so that the high-temperature suspensibility is influenced, and the particle size is increased, and the inventor finds that when the intermediate hydrophilic and the double-end hydrophobic bis-stearamide and the comb-shaped polycarboxylate are added and the anionic and non-active groups are contained, the anionic polycarboxylate and the fatty alcohol polyoxyethylene phosphate are utilized to jointly act, the hydrophobic stearamide structures at the two ends promote the hydrophobic effect while the charge is adsorbed by the charge, and the charge is dispersed and repelled by the NH structures, and the magnesium aluminum silicate is subjected to adsorption exchange, so that the high-temperature suspensibility is improved, the system viscosity is reduced, and the pouring residue is prevented from increasing.
The inventor also finds that when the polycarboxylate with multiple adsorption sites is used for acting, the fatty alcohol polyoxyethylene phosphate with lower EO number and better lipophilicity is used for acting, so that the density and the thickness of an adsorption film of the active ingredient can be further increased, and the action of different anionic charges is further beneficial to the action of stearamide and magnesium aluminum silicate, and the pouring efficiency is promoted.
Preferably, the wetting agent is selected from one or more of polyether polyester modified organic siloxane, EO-PO block polyether, methyl phenol formaldehyde resin, sodium dodecyl sulfate, polyoxyethylene ether and dioctyl sodium sulfosuccinate.
Preferably, the wetting agent comprises a polyether polyester modified organosiloxane and an EO-PO block polyether in a weight ratio of (0.8 to 1.5): 1.
in a preferred embodiment, the viscosity of the polyether polyester modified organosiloxane at 25 ℃ is 1000 to 5000cps, such as polyether polyester co-modified polysiloxane 8244 (viscosity at 25 ℃ is 1000 to 5000 cps) from Shanghai Raman reagent, inc.
In a preferred embodiment, the number average molecular weight of the EO-PO block polyether is 3000 to 4500, and as examples of the EO-PO block polyether, number average molecular weights of 3100, 3500, and 4100 are enumerated.
The EO-PO block polyether having a number average molecular weight of 3100 was purchased from Pasteur, germany under the type Pluronic RPE 2520.
The EO-PO block polyether having a number average molecular weight of 3500 was purchased from Pasteur, germany under the type Pluronic RPE 3100.
The EO-PO block polyether having a number average molecular weight of 4100 was purchased from Pasov Germany and was designated Pluronic RPE 1720
The inventors found that, when an anionic polycarboxylate and a fatty alcohol polyoxyethylene ether phosphate are added as the dispersant, the persistent foaming property is difficult to be reduced because of the higher foaming property of the anionic dispersant, while the inventors found that, when a polyether polyester-modified organosiloxane and an EO-PO block polyether are added, the poor affinity of the siloxane and PO blocks and water is utilized to reduce particle aggregation and creaming while simultaneously enabling easy action at the foam interface, reduce the combination of foam and foam formed by the polycarboxylate and the like, promote foam reduction, and obtain a suspension having low foaming and low persistent foaming properties.
And the inventors also found that when polyether polyester modified organosiloxane is simply added, although surface tension can be reduced, it is difficult to sufficiently combine with polycarboxylate to rapidly reduce the amount of foam, and rapid defoaming is promoted by adding a block and modified organosiloxane to work together.
Preferably, the thickening agent is selected from one or more of magnesium aluminum silicate, urea, sodium alginate, xanthan gum, sodium carboxymethylcellulose and sodium alginate.
Preferably, the thickening agent comprises magnesium aluminium silicate and xanthan gum.
Preferably, the preparation raw materials of the spinosad suspending agent further comprise 0.05-0.5wt% of preservative, 0.01-0.5wt% of defoaming agent and 4-8wt% of antifreeze agent in percentage by weight.
Preferably, the preservative is selected from one or more of propionic acid and its sodium salt, 1, 2-benzisothiazolinone, isothiazolinone, sodium benzoate, methyl p-hydroxy phenyl ester.
Preferably, the defoaming agent is selected from one or more of fatty acid esters, polyethers, polydimethylsiloxane, long-chain fatty alcohol and tributyl phosphate.
Preferably, the antifreeze agent is ethylene glycol or 1, 2-propylene glycol.
The invention provides a preparation method of a spinosad suspending agent in a second aspect, which comprises the following steps:
and mixing, shearing, dispersing and grinding the preparation raw materials of the spinosad suspending agent to obtain the spinosad suspending agent.
Preferably, the preparation method of the spinosad suspending agent comprises the following steps:
s1, mixing a thickening agent and an anti-freezing agent for later use;
s2, adding water, a dispersing agent, a wetting agent, a preservative and a defoaming agent into a shearing device for dispersing to obtain a mixture a;
s3, putting spinosad and the component B into a shearing device to be mixed and dispersed with the mixture a, adding a mixed solution of a thickening agent and an anti-freezing agent to be dispersed, and adding the dispersed mixture into a sand mill to be sanded;
and S4, adding the mixture into a mixing kettle after sanding is finished, and adding a defoaming agent to prepare the spinosad suspending agent.
Further, the preparation method of the spinosad suspending agent comprises the following steps:
s1, mixing xanthan gum and ethylene glycol to obtain a mixed solution;
s2, adding water, fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate, vinyl bis-stearamide, polyether polyester modified organosiloxane, EO-PO block polyether, 1, 2-benzisothiazolinone and 1/2 of polydimethylsiloxane by weight into a shearing device for dispersing to obtain a mixture a;
s3, putting spinosad and the component B into a shearing device to be mixed and dispersed with the mixture a, adding a mixed solution of magnesium aluminum silicate, xanthan gum and ethylene glycol to be dispersed, and adding the dispersed mixture into a sand mill to be sanded;
and S4, adding the mixture into a mixing kettle after sanding is finished, and adding the rest of polydimethylsiloxane to prepare the spinosad suspending agent.
Preferably, the S4 sand is ground to control the grain diameter D90 to be less than 3.0um.
The inventor finds that the thickening agent such as magnesium aluminum silicate and xanthan gum is added in the sanding process to promote the uniform particle size of the active ingredient in the sanding process and form stable micelle adhesion, but the inventor also finds that the large structure and water absorption of magnesium aluminum silicate and xanthan gum affect the internal water absorption and form non-uniform agglomerates, thereby affecting the particle uniformity and micelle adhesion in the sanding process, and the invention can promote the internal water absorption and expansion of the thickening agent while promoting the external water absorption and expansion of the thickening agent by mixing the thickening agent and an appropriate amount of antifreeze agent and adding the thickening agent and the antifreeze agent into a suspension system, thereby being beneficial to the stabilization of the particle size and micelle structure after sanding and reducing the particle growth in the storage process, and the inventor finds that the D50 particle size is increased after being stored for 14 days when the thickening agent and the antifreeze agent are added respectively.
The third aspect of the invention provides an application of a spinosad suspending agent in the technical field of pesticide disinsection.
Advantageous effects
In the invention, the EO-PO block polyether and polyether polyester are selected to modify organic siloxane, so that the prepared spinosad suspending agent has good low-foaming and low-lasting foaming properties in the application process.
According to the invention, vinyl distearamide, fatty alcohol polyoxyethylene ether phosphate and anionic polycarboxylate are selected as dispersing agents, so that the suspension has good suspension performance in the application process along with the increase of storage time, especially at a higher temperature, and the increase of pouring residues can be avoided.
According to the invention, the aluminum magnesium silicate and the xanthan gum are selected as the thickening agents, and the glycol is added as the antifreeze agent, so that the sanding stability can be promoted, and the particle size stability in the storage process can be improved.
The spinosad suspension prepared by compounding the spinosad with chlorantraniliprole, indoxacarb and methoxyfenozide has a good sterilization effect, the sterilization spectrum is expanded, and pesticide residues and drug resistance are avoided.
The spinosad, chlorantraniliprole, indoxacarb and methoxyfenozide are compounded in different proportions, so that the obtained spinosad suspending agent has the spinosad suspending agent, the prepared spinosad suspending agent has a good insecticidal effect, particularly, the agricultural lepidoptera pests such as cotton bollworm, plutella xylostella, cabbage caterpillar, beet noctuid, prodenia litura, cabbage prodenia enge and the like have excellent insecticidal activity, particularly, the compound use of the spinosad and the cabbage prodenia litura is beneficial to delaying the generation of drug resistance of the moths, prolonging the service life of pesticide varieties, reducing the use dosage, saving the cost, reducing the pollution to the environment, and having better application value in the aspects of drug resistance and comprehensive control of the prodenia litura and the cabbage prodenia litura.
Drawings
Fig. 1-10 are contents of a method for indoor toxicity determination of cabbage prodenia litura by a spinosad suspending agent.
FIGS. 11-19 are contents of the method for indoor toxicity determination of cabbage prodenia litura by spinosad suspending agents.
FIGS. 20-27 are the contents of the method for indoor virulence determination of Spodoptera litura with spinosad suspending agents.
Detailed Description
Example 1
The spinosad suspending agent is prepared from the following raw materials in percentage by weight: 11.12wt% of spinosad, 8wt% of dispersant, 2wt% of wetting agent, 1.15wt% of thickener, 0.1wt% of defoamer, 0.15wt% of preservative, 6wt% of antifreeze and the balance of water.
The CAS number of the spinosad is 131929-60-7.
The dispersing agent consists of fatty alcohol polyoxyethylene ether phosphate, anionic polycarboxylate and vinyl bis stearamide.
The weight ratio of the fatty alcohol-polyoxyethylene ether phosphate to the anionic polycarboxylate to the vinyl bis stearamide is 4.
The fatty alcohol-polyoxyethylene ether phosphate is C12-14 fatty alcohol-polyoxyethylene ether phosphate, and the purchase manufacturer is a chemical technology company Limited in Cao of North Hu east, and the model is AEO-3P.
The anionic polycarboxylate was purchased from Hensman USA under the TER-SPERSE 2700 model.
The CAS number of the vinyl bis-stearamide is 110-30-5.
The wetting agent consists of polyether polyester modified organic siloxane and EO-PO block polyether, and the weight ratio of the polyether polyester modified organic siloxane to the EO-PO block polyether is 1:1.
the polyether polyester modified organic siloxane is polyether polyester copolymerization modified polysiloxane 8244 of Shanghai Raman reagent company Limited.
The EO-PO block polyether was purchased from Pasteur, germany and was designated as Pluronic RPE 3100.
The thickening agent comprises magnesium aluminum silicate and xanthan gum, wherein the weight ratio of the magnesium aluminum silicate to the xanthan gum is 1: 0.15.
The purchasing manufacturer of the magnesium aluminum silicate is Jinan Yingsheng chemical technology limited company, and the content of effective components is 99 percent.
The xanthan gum purchasing manufacturer is Shenzhen Lefu biotechnology limited, and the brand is MuyuvON.
The defoaming agent is polydimethylsiloxane.
The polydimethylsiloxane is purchased from Hubei New Sihai chemical industry Co., ltd, and the specification is 20/200.
The preservative is 1, 2-benzisothiazolinone.
The CAS number of the 1, 2-benzisothiazolinone is 2634-33-5.
The antifreeze agent is ethylene glycol.
The invention provides a preparation method of a spinosad suspending agent in a second aspect, which comprises the following steps:
s1, mixing xanthan gum and ethylene glycol to obtain a mixed solution;
s2, adding water, fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate, vinyl bis-stearamide, polyether polyester modified organosiloxane, EO-PO block polyether, 1, 2-benzisothiazolinone and 1/2 of polydimethylsiloxane by weight into a shearing pot for shearing and dispersing to obtain a mixture a;
s3, putting spinosad in a shearing device, mixing and dispersing with the mixture a, adding a mixed solution of magnesium aluminum silicate, xanthan gum and glycol for dispersing, and adding the dispersed mixture into a sand mill for sanding to obtain a mixture b;
and S4, finishing sanding when the D90 particle size of the mixture b is smaller than 3.0um, adding the mixture b into a mixing kettle, and adding the rest polydimethylsiloxane to prepare the spinosad suspending agent.
The third aspect of the invention provides an application of a spinosad suspending agent in the technical field of pesticide disinsection.
Example 2
The spinosad suspending agent is prepared from the following raw materials in percentage by weight: 11.12wt% of component B, 8wt% of dispersant, 2wt% of wetting agent, 1.15wt% of thickener, 0.1wt% of defoamer, 0.15wt% of preservative, 6wt% of antifreeze agent and the balance of water.
The component B is chlorantraniliprole.
The CAS number of the chlorantraniliprole is 500008-45-7.
The dispersing agent consists of fatty alcohol polyoxyethylene ether phosphate, anionic polycarboxylate and vinyl bis stearamide.
The weight ratio of the fatty alcohol-polyoxyethylene ether phosphate to the anionic polycarboxylate to the vinyl bis stearamide is 4.
The fatty alcohol-polyoxyethylene ether phosphate is C12-14 fatty alcohol-polyoxyethylene ether phosphate, and the purchase manufacturer is a chemical technology company Limited in Cao of North Hu east, and the model is AEO-3P.
The anionic polycarboxylate was purchased from Hensman USA under the TER-SPERSE 2700 model.
The CAS number of the vinyl bis-stearamide is 110-30-5.
The wetting agent consists of polyether polyester modified organic siloxane and EO-PO block polyether, and the weight ratio of the polyether polyester modified organic siloxane to the EO-PO block polyether is 1:1.
the polyether polyester modified organic siloxane is polyether polyester copolymerization modified polysiloxane 8244 of Shanghai Raman reagent company Limited.
The EO-PO block polyether was purchased from Pasteur, germany and was designated as Pluronic RPE 3100.
The thickening agent comprises magnesium aluminum silicate and xanthan gum, wherein the weight ratio of the magnesium aluminum silicate to the xanthan gum is 1: 0.15.
The purchasing manufacturer of the magnesium aluminum silicate is Jinan Yingsheng chemical technology limited company, and the content of effective components is 99 percent.
The xanthan gum purchasing manufacturer is Shenzhen Lefu biotechnology limited company, and the brand is MuyuvON.
The defoaming agent is polydimethylsiloxane.
The polydimethylsiloxane is purchased from Hubei New Sihai chemical industry Co., ltd, and the specification is 20/200.
The preservative is 1, 2-benzisothiazolinone.
The CAS number of the 1, 2-benzisothiazolinone is 2634-33-5.
The antifreeze agent is ethylene glycol.
The invention provides a preparation method of a spinosad suspending agent in a second aspect, which comprises the following steps:
s1, mixing xanthan gum and ethylene glycol to obtain a mixed solution;
s2, adding water, fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate, vinyl bis stearamide, polyether polyester modified organosiloxane, EO-PO block polyether, 1, 2-benzisothiazolinone and 1/2 of polydimethylsiloxane by weight into a shearing pot for shearing and dispersing to obtain a mixture a;
s3, adding chlorantraniliprole into a shearing device, mixing and dispersing the chlorantraniliprole with the mixture a, adding a mixed solution of magnesium aluminum silicate, xanthan gum and ethylene glycol for dispersing, and adding the mixture into a sand mill for sanding to obtain a mixture b after dispersing;
and S4, finishing sanding when the particle size of D90 of the mixture b is smaller than 3.0um, adding the mixture b into a mixing kettle, and adding the rest polydimethylsiloxane to prepare the spinosad suspending agent.
The third aspect of the invention provides an application of a spinosad suspending agent in the technical field of pesticide disinsection.
Example 3
The spinosad suspending agent is prepared from the following raw materials in percentage by weight: 11.12wt% of component B, 8wt% of dispersant, 2wt% of wetting agent, 1.15wt% of thickener, 0.1wt% of defoamer, 0.15wt% of preservative, 6wt% of antifreeze agent and the balance of water.
The component B is indoxacarb.
The CAS number of the indoxacarb is 144171-61-9.
The dispersing agent consists of fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate and vinyl bis stearamide.
The weight ratio of the fatty alcohol-polyoxyethylene ether phosphate to the anionic polycarboxylate to the vinyl bis stearamide is 4.
The fatty alcohol-polyoxyethylene ether phosphate is C12-14 fatty alcohol-polyoxyethylene ether phosphate, and the purchase manufacturer is a chemical technology company Limited in Cao of North Hu east, and the model is AEO-3P.
The anionic polycarboxylate was purchased from Hensman USA under the TER-SPERSE 2700 model.
The CAS number of the vinyl bis-stearamide is 110-30-5.
The wetting agent consists of polyether polyester modified organic siloxane and EO-PO block polyether, and the weight ratio of the polyether polyester modified organic siloxane to the EO-PO block polyether is 1:1.
the polyether polyester modified organic siloxane is polyether polyester copolymerization modified polysiloxane 8244 of Shanghai Raman reagent company Limited.
The EO-PO block polyether was purchased from Pasteur, germany and was designated as Pluronic RPE 3100.
The thickening agent comprises magnesium aluminum silicate and xanthan gum, wherein the weight ratio of the magnesium aluminum silicate to the xanthan gum is 1: 0.15.
The purchasing manufacturer of the magnesium aluminum silicate is Jinan Yingsheng chemical technology limited company, and the content of effective components is 99 percent.
The xanthan gum purchasing manufacturer is Shenzhen Lefu biotechnology limited, and the brand is MuyuvON.
The defoaming agent is polydimethylsiloxane.
The polydimethylsiloxane is purchased from Hubei New Sihai chemical industry Co., ltd, and the specification is 20/200.
The preservative is 1, 2-benzisothiazolinone.
The CAS number of the 1, 2-benzisothiazolinone is 2634-33-5.
The antifreeze agent is glycol.
The invention provides a preparation method of a spinosad suspending agent in a second aspect, which comprises the following steps:
s1, mixing xanthan gum and ethylene glycol to obtain a mixed solution;
s2, adding water, fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate, vinyl bis-stearamide, polyether polyester modified organosiloxane, EO-PO block polyether, 1, 2-benzisothiazolinone and 1/2 of polydimethylsiloxane by weight into a shearing pot for shearing and dispersing to obtain a mixture a;
s3, putting indoxacarb into a shearing device, mixing and dispersing the indoxacarb with the mixture a, adding a mixed solution of magnesium aluminum silicate, xanthan gum and ethylene glycol for dispersing, and adding the mixture into a sand mill for sanding after dispersing to obtain a mixture b;
and S4, finishing sanding when the D90 particle size of the mixture b is smaller than 3.0um, adding the mixture b into a mixing kettle, and adding the rest polydimethylsiloxane to prepare the spinosad suspending agent.
The third aspect of the invention provides an application of a spinosad suspending agent in the technical field of pesticide disinsection.
Example 4
The spinosad suspending agent is prepared from the following raw materials in percentage by weight: 11.12wt% of component B, 8wt% of dispersant, 2wt% of wetting agent, 1.15wt% of thickener, 0.1wt% of defoamer, 0.15wt% of preservative, 6wt% of antifreeze agent and the balance of water.
The component B is methoxyfenozide.
The CAS number of the methoxyfenozide is 161050-58-4.
The dispersing agent consists of fatty alcohol polyoxyethylene ether phosphate, anionic polycarboxylate and vinyl bis stearamide.
The weight ratio of the fatty alcohol-polyoxyethylene ether phosphate to the anionic polycarboxylate to the vinyl bis stearamide is 4.
The fatty alcohol-polyoxyethylene ether phosphate is C12-14 fatty alcohol-polyoxyethylene ether phosphate, and the purchase manufacturer is a chemical technology company Limited in Cao of North Hu east, and the model is AEO-3P.
The anionic polycarboxylate was purchased from Hensman USA under the TER-SPERSE 2700 model.
The CAS number of the vinyl bis-stearamide is 110-30-5.
The wetting agent consists of polyether polyester modified organic siloxane and EO-PO block polyether, and the weight ratio of the polyether polyester modified organic siloxane to the EO-PO block polyether is 1:1.
the polyether polyester modified organic siloxane is polyether polyester copolymerization modified polysiloxane 8244 of Shanghai Raman reagent company Limited.
The EO-PO block polyether was purchased from Pasteur, germany and was designated as Pluronic RPE 3100.
The thickening agent comprises magnesium aluminum silicate and xanthan gum, wherein the weight ratio of the magnesium aluminum silicate to the xanthan gum is 1: 0.15.
The purchasing manufacturer of the magnesium aluminum silicate is Jinan Yingsheng chemical technology limited company, and the content of effective components is 99 percent.
The xanthan gum purchasing manufacturer is Shenzhen Lefu biotechnology limited, and the brand is MuyuvON.
The defoaming agent is polydimethylsiloxane.
The polydimethylsiloxane is purchased from Hubei New Sihai chemical industry Co., ltd, and the specification is 20/200.
The preservative is 1, 2-benzisothiazolinone.
The CAS number of the 1, 2-benzisothiazolinone is 2634-33-5.
The antifreeze agent is ethylene glycol.
The invention provides a preparation method of a spinosad suspending agent in a second aspect, which comprises the following steps:
s1, mixing xanthan gum and ethylene glycol to obtain a mixed solution;
s2, adding water, fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate, vinyl bis-stearamide, polyether polyester modified organosiloxane, EO-PO block polyether, 1, 2-benzisothiazolinone and 1/2 of polydimethylsiloxane by weight into a shearing pot for shearing and dispersing to obtain a mixture a;
s3, putting methoxyfenozide into a shearing device, mixing and dispersing with the mixture a, adding a mixed solution of magnesium aluminum silicate, xanthan gum and ethylene glycol for dispersing, and adding into a sand mill for sanding after dispersing to obtain a mixture b;
and S4, finishing sanding when the particle size of D90 of the mixture b is smaller than 3.0um, adding the mixture b into a mixing kettle, and adding the rest polydimethylsiloxane to prepare the spinosad suspending agent.
The third aspect of the invention provides an application of a spinosad suspending agent in the technical field of pesticide disinsection.
Example 5
The spinosad suspending agent is prepared from the following raw materials in percentage by weight: 11.12wt% of spinosad, a component B, 8wt% of a dispersant, 2wt% of a wetting agent, 1.15wt% of a thickening agent, 0.1wt% of a defoaming agent, 0.15wt% of a preservative, 6wt% of an antifreeze agent and the balance of water.
The weight ratio of the spinosad to the component B is 5:1.
the CAS number of the spinosad is 131929-60-7.
The component B is chlorantraniliprole.
The CAS number of the chlorantraniliprole is 500008-45-7.
The dispersing agent consists of fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate and vinyl bis stearamide.
The weight ratio of the fatty alcohol-polyoxyethylene ether phosphate to the anionic polycarboxylate to the vinyl bis stearamide is 4.
The fatty alcohol-polyoxyethylene ether phosphate is C12-14 fatty alcohol-polyoxyethylene ether phosphate, and the purchase manufacturer is a product of AEO-3P of northHubei Dongcao chemical science and technology Limited.
The anionic polycarboxylate was purchased from Hensman USA under the TER-SPERSE 2700 model.
The CAS number of the vinyl bis-stearamide is 110-30-5.
The wetting agent consists of polyether polyester modified organic siloxane and EO-PO block polyether, and the weight ratio of the polyether polyester modified organic siloxane to the EO-PO block polyether is 1:1.
the polyether polyester modified organic siloxane is polyether polyester copolymerization modified polysiloxane 8244 of Shanghai Raman reagent company Limited.
The EO-PO block polyether was purchased from Pasteur, germany and was designated as Pluronic RPE 3100.
The thickening agent comprises magnesium aluminum silicate and xanthan gum, wherein the weight ratio of the magnesium aluminum silicate to the xanthan gum is 1: 0.15.
The purchasing manufacturer of the magnesium aluminum silicate is Jinan Yingsheng chemical technology limited company, and the content of effective components is 99 percent.
The xanthan gum purchasing manufacturer is Shenzhen Lefu biotechnology limited, and the brand is MuyuvON.
The defoaming agent is polydimethylsiloxane.
The polydimethylsiloxane is purchased from Hubei New Sihai chemical industry Co., ltd, and the specification is 20/200.
The preservative is 1, 2-benzisothiazolinone.
The CAS number of the 1, 2-benzisothiazolinone is 2634-33-5.
The antifreeze agent is ethylene glycol.
The invention provides a preparation method of a spinosad suspending agent in a second aspect, which comprises the following steps:
s1, mixing xanthan gum and ethylene glycol to obtain a mixed solution;
s2, adding water, fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate, vinyl bis-stearamide, polyether polyester modified organosiloxane, EO-PO block polyether, 1, 2-benzisothiazolinone and 1/2 of polydimethylsiloxane by weight into a shearing pot for shearing and dispersing to obtain a mixture a;
s3, putting spinosad and chlorantraniliprole into a shearing device, mixing and dispersing the spinosad and the chlorantraniliprole with the mixture a, adding a mixed solution of magnesium aluminum silicate, xanthan gum and glycol for dispersing, and adding the mixture into a sand mill for sanding after dispersing to obtain a mixture b;
and S4, finishing sanding when the particle size of D90 of the mixture b is smaller than 3.0um, adding the mixture b into a mixing kettle, and adding the rest polydimethylsiloxane to prepare the spinosad suspending agent.
The third aspect of the invention provides an application of a spinosad suspending agent in the technical field of pesticide disinsection.
Example 6
Example 6 provides a spinosyn suspension, which differs from example 5 in that the weight ratio of spinosyn to chlorantraniliprole in example 6 is 3:1.
example 7
Example 7 provides a spinosyn suspension, differing from example 5 in that the weight ratio of spinosyn to chlorantraniliprole in example 7 is 1:1.
example 8
Example 8 provides a spinosyn suspension, which differs from example 5 in that the weight ratio of spinosyn to chlorantraniliprole in example 8 is 1:3.
example 9
Example 9 provides a spinosyn suspension, differing from example 5 in that the weight ratio of spinosyn to chlorantraniliprole in example 9 is 1:5.
example 10
The spinosad suspending agent is prepared from the following raw materials in percentage by weight: 11.12wt% of spinosad, a component B, 8wt% of a dispersant, 2wt% of a wetting agent, 1.15wt% of a thickening agent, 0.1wt% of a defoaming agent, 0.15wt% of a preservative, 6wt% of an antifreeze agent and the balance of water.
The weight ratio of the spinosad to the component B is 3:1.
the CAS number of the spinosad is 131929-60-7.
The component B is indoxacarb.
The CAS number of the indoxacarb is 144171-61-9.
The dispersing agent consists of fatty alcohol polyoxyethylene ether phosphate, anionic polycarboxylate and vinyl bis stearamide.
The weight ratio of the fatty alcohol-polyoxyethylene ether phosphate to the anionic polycarboxylate to the vinyl bis stearamide is 4.
The fatty alcohol-polyoxyethylene ether phosphate is C12-14 fatty alcohol-polyoxyethylene ether phosphate, and the purchase manufacturer is a chemical technology company Limited in Cao of North Hu east, and the model is AEO-3P.
The anionic polycarboxylate was purchased from Hensman USA under the TER-SPERSE 2700 model.
The CAS number of the vinyl bis-stearamide is 110-30-5.
The wetting agent consists of polyether polyester modified organic siloxane and EO-PO block polyether, and the weight ratio of the polyether polyester modified organic siloxane to the EO-PO block polyether is 1:1.
the polyether polyester modified organic siloxane is polyether polyester copolymerization modified polysiloxane 8244 of Shanghai Raman reagent company.
The EO-PO block polyether was purchased from Pasteur, germany and was designated as Pluronic RPE 3100.
The thickening agent comprises magnesium aluminum silicate and xanthan gum, wherein the weight ratio of the magnesium aluminum silicate to the xanthan gum is 1: 0.15.
The purchasing manufacturer of the magnesium aluminum silicate is Jinan Yingsheng chemical technology limited company, and the content of effective components is 99 percent.
The xanthan gum purchasing manufacturer is Shenzhen Lefu biotechnology limited, and the brand is MuyuvON.
The defoaming agent is polydimethylsiloxane.
The polydimethylsiloxane is purchased from Hubei New Sihai chemical industry Co., ltd, and the specification is 20/200.
The preservative is 1, 2-benzisothiazolinone.
The CAS number of the 1, 2-benzisothiazolinone is 2634-33-5.
The antifreeze agent is ethylene glycol.
The invention provides a preparation method of a spinosad suspending agent in a second aspect, which comprises the following steps:
s1, mixing xanthan gum and ethylene glycol to obtain a mixed solution;
s2, adding water, fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate, vinyl bis stearamide, polyether polyester modified organosiloxane, EO-PO block polyether, 1, 2-benzisothiazolinone and 1/2 of polydimethylsiloxane by weight into a shearing pot for shearing and dispersing to obtain a mixture a;
s3, putting spinosad and indoxacarb into a shearing device, mixing and dispersing the spinosad and the indoxacarb with the mixture a, adding a mixed solution of magnesium aluminum silicate, xanthan gum and ethylene glycol for dispersing, and adding the mixture into a sand mill for sanding after dispersing to obtain a mixture b;
and S4, finishing sanding when the D90 particle size of the mixture b is smaller than 3.0um, adding the mixture b into a mixing kettle, and adding the rest polydimethylsiloxane to prepare the spinosad suspending agent.
The third aspect of the invention provides an application of a spinosad suspending agent in the technical field of pesticide disinsection.
Example 11
Example 11 provides a spinosad suspension, which is different from example 10 in that the weight ratio of spinosad to indoxacarb in example 11 is 1:1.
example 12
Example 12 provides a spinosad suspension, which is different from example 10 in that the weight ratio of spinosad to indoxacarb in example 12 is 1:2.
example 13
Example 13 provides a spinosad suspension, which is different from example 10 in that the weight ratio of spinosad to indoxacarb in example 13 is 1:3.
example 14
Example 14 provides a spinosad suspension, which is different from example 10 in that the weight ratio of spinosad to indoxacarb in example 14 is 1:4.
example 15
Example 15 provides a spinosad suspension, which is different from example 10 in that the weight ratio of spinosad to indoxacarb in example 15 is 1:5.
example 16
Example 16 provides a spinosad suspension, which is different from example 10 in that the weight ratio of spinosad to indoxacarb in example 16 is 1:7.
example 17
Example 17 provides a spinosad suspension, which is different from example 10 in that the weight ratio of spinosad to indoxacarb in example 17 is 1:9.
example 18
The spinosad suspending agent is prepared from the following raw materials in percentage by weight: 11.12wt% of spinosad, a component B, 8wt% of a dispersant, 2wt% of a wetting agent, 1.15wt% of a thickening agent, 0.1wt% of a defoaming agent, 0.15wt% of a preservative, 6wt% of an antifreeze agent and the balance of water.
The weight ratio of the spinosad to the component B is 5:1.
the CAS number of the spinosad is 131929-60-7.
The component B is methoxyfenozide.
The CAS number of the methoxyfenozide is 161050-58-4.
The dispersing agent consists of fatty alcohol polyoxyethylene ether phosphate, anionic polycarboxylate and vinyl bis stearamide.
The weight ratio of the fatty alcohol-polyoxyethylene ether phosphate to the anionic polycarboxylate to the vinyl bis stearamide is 4.
The fatty alcohol-polyoxyethylene ether phosphate is C12-14 fatty alcohol-polyoxyethylene ether phosphate, and the purchase manufacturer is a chemical technology company Limited in Cao of North Hu east, and the model is AEO-3P.
The anionic polycarboxylate was purchased from Hensman USA under the TER-SPERSE 2700 model.
The CAS number of the vinyl bis-stearamide is 110-30-5.
The wetting agent consists of polyether polyester modified organic siloxane and EO-PO block polyether, and the weight ratio of the polyether polyester modified organic siloxane to the EO-PO block polyether is 1:1.
the polyether polyester modified organic siloxane is polyether polyester copolymerization modified polysiloxane 8244 of Shanghai Raman reagent company Limited.
The EO-PO block polyether was purchased from Pasteur, germany and was designated as Pluronic RPE 3100.
The thickening agent comprises magnesium aluminum silicate and xanthan gum, wherein the weight ratio of the magnesium aluminum silicate to the xanthan gum is 1: 0.15.
The purchasing manufacturer of the magnesium aluminum silicate is Jinan Yingsheng chemical technology limited company, and the content of effective components is 99 percent.
The xanthan gum purchasing manufacturer is Shenzhen Lefu biotechnology limited company, and the brand is MuyuvON.
The defoaming agent is polydimethylsiloxane.
The polydimethylsiloxane is purchased from Hubei New Sihai chemical industry Co., ltd, and the specification is 20/200.
The preservative is 1, 2-benzisothiazolinone.
The CAS number of the 1, 2-benzisothiazolinone is 2634-33-5.
The antifreeze agent is ethylene glycol.
The invention provides a preparation method of a spinosad suspending agent in a second aspect, which comprises the following steps:
s1, mixing xanthan gum and ethylene glycol to obtain a mixed solution;
s2, adding water, fatty alcohol-polyoxyethylene ether phosphate, anionic polycarboxylate, vinyl bis-stearamide, polyether polyester modified organosiloxane, EO-PO block polyether, 1, 2-benzisothiazolinone and 1/2 of polydimethylsiloxane by weight into a shearing pot for shearing and dispersing to obtain a mixture a;
s3, putting spinosad and methoxyfenozide into a shearing device to be mixed and dispersed with the mixture a, adding a mixed solution of magnesium aluminum silicate, xanthan gum and ethylene glycol to be dispersed, and adding the dispersed mixture into a sand mill to be subjected to sand milling to obtain a mixture b;
and S4, finishing sanding when the D90 particle size of the mixture b is smaller than 3.0um, adding the mixture b into a mixing kettle, and adding the rest polydimethylsiloxane to prepare the spinosad suspending agent.
The third aspect of the invention provides an application of a spinosad suspending agent in the technical field of pesticide disinsection.
Example 19
Example 19 provides a spinosyn suspension, differing from example 18 in that the weight ratio of spinosyn to methoxyfenozide in example 19 is 3:1.
example 20
Example 20 provides a spinosyn suspension, differing from example 18 in that the weight ratio of spinosyn to methoxyfenozide in example 20 is 1:1.
example 21
Example 21 provides a spinosyn suspension, differing from example 18 in that the weight ratio of spinosyn to methoxyfenozide in example 21 is 1:2.
example 22
Example 22 provides a spinosyn suspension, which differs from example 18 in that the weight ratio of spinosyn to methoxyfenozide in example 22 is 1:3.
example 23
Example 23 provides a spinosyn suspension, differing from example 18 in that the weight ratio of spinosyn to methoxyfenozide in example 23 is 1:4.
example 24
Example 24 provides a spinosyn suspension, differing from example 18 in that the weight ratio of spinosyn to methoxyfenozide in example 24 is 1:5.
example 25
Example 25 provides a spinosyn suspension, which differs from example 14 in that no EO-PO block polyether is added to the raw materials for its preparation.
Example 26
Example 26 provides a spinosyn suspension, which differs from example 14 in that no fatty alcohol polyoxyethylene ether phosphate is added to the raw materials for preparing the spinosyn suspension.
Performance testing
1. Indoor toxicity test:
indoor toxicity of the spinosad suspending agent prepared in the embodiment 1, the embodiment 2 and the embodiments 5-9 on cabbage prodenia litura is determined, and the determination result is shown in table 1; the test methods and analysis of the results are shown in FIGS. 1-9.
TABLE 1
Figure RE-GDA0003609491930000181
Indoor toxicity of the spinosad suspending agent prepared in the embodiment 1, the embodiment 3 and the embodiments 10-17 on cabbage prodenia litura is determined, and the determination result is shown in a table 2; the test methods and analysis of the results are shown in FIGS. 10-18.
TABLE 2
Figure RE-GDA0003609491930000182
Figure RE-GDA0003609491930000191
Indoor toxicity of the spinosad suspending agents prepared in the embodiment 1, the embodiment 4 and the embodiments 18-24 to prodenia litura is determined, and the determination results are shown in a table 3; the test methods and analysis of the results are shown in FIGS. 19-27.
TABLE 3
Figure RE-GDA0003609491930000192
2. Heat storage, retroversion test of heat storage
The test method comprises the following steps: the pourability test was carried out according to the test method in GB/T31737-2015 method for measuring pourability of pesticides.
Test samples: the spinosyn suspensions prepared in example 7, example 14, example 18, example 25 and example 26 were tested before and after hot-storage, respectively, after hot-storage for 14 days according to GBT 19136-2003 method for determining the stability of pesticides to hot-storage at 54 ℃, and the test results are shown in Table 4.
3. Heat storage, long-lasting foamability test after Heat storage
The persistent foaming test was carried out according to the test method of GBT 28137-2011 method for determining persistent foaming of pesticides.
Test samples: the spinosyn suspensions prepared in example 7, example 14, example 18, example 25 and example 26 were tested before and after heat storage at 54 ℃ for 14 days according to GBT 19136-2003 method for determining the heat storage stability of pesticides after heat storage, and the test results are shown in Table 4.
TABLE 4
Figure RE-GDA0003609491930000201
4. Particle size, suspension, wet sieve test
And (3) suspension rate determination: weighing 1.0g of sample (accurate to 0.0002 g), completely transferring the rest 25mL of suspension obtained by the method of '4.2' in GB/T14825-2006 into a 50mL volumetric flask, fixing the volume to the scale by using methanol, dissolving the sample by ultrasonic oscillation for 5min, cooling to room temperature, shaking up, accurately sucking the sample into the 5mL to 50mL volumetric flask by using a pipette, diluting to the scale by using methanol, shaking up, filtering, analyzing by liquid chromatography to obtain the mass of the active ingredients of spinosad and the component B, and calculating the suspension rate.
The wet sieve passing rate was measured according to the test method of GB/T16150-1995 method for measuring the fineness of agricultural chemicals and wettable powders.
The particle size was measured using a laser particle size analyzer and the results are shown in table 5.
Test samples: the spinosyn suspension prepared in example 14 was stored at 54 ℃ for 14 days before and after hot storage according to GBT 19136-2003 method for determining the thermal storage stability of pesticides after hot storage, and the test results are shown in Table 5.
TABLE 5
Figure RE-GDA0003609491930000202

Claims (10)

1. The spinosad suspending agent is characterized in that the preparation raw materials of the spinosad suspending agent comprise spinosad and a component B, wherein the component B is one or more selected from chlorantraniliprole, indoxacarb and methoxyfenozide.
2. The spinosyn suspension of claim 1, wherein the weight ratio of spinosyn to chlorantraniliprole is (1-5): (1-5).
3. The spinosyn suspension of claim 1, wherein the weight ratio of spinosad to indoxacarb is (1-3): (1-9).
4. The spinosyn suspension of claim 1, wherein the weight ratio of spinosyn to methoxyfenozide is (1-5): (1-5).
5. The spinosyn suspension of any of claims 1-4, wherein the spinosyn suspension is prepared from raw materials comprising a dispersant, a wetting agent, a thickener, and water.
6. The spinosyn suspension of claim 5, wherein the wetting agent is selected from one or more of polyether polyester modified organosiloxanes, EO-PO block polyethers, methyl phenol formaldehyde resins, sodium dodecyl sulfate, polyoxyethylene ethers, dioctyl sodium sulfosuccinate.
7. The spinosyn suspension of claim 5, wherein the dispersing agent is selected from one or more of fatty alcohol polyoxyethylene ether phosphate, calcium lignosulfonate, anionic polycarboxylate, sodium methylenedinaphthalene sulfonate, vinyl bisstearamide, alkyl naphthalene sulfonate formaldehyde condensate.
8. The spinosad suspension formulation of claim 5, wherein the preparation raw materials of the spinosad suspension formulation further comprise a preservative, a defoaming agent and an antifreeze.
9. A method of preparing a spinosyn suspension of any of claims 5-8, comprising the steps of:
and mixing, shearing, dispersing and grinding the preparation raw materials of the spinosad suspending agent to obtain the spinosad suspending agent.
10. Use of a spinosyn suspension according to any of claims 1-8 for combating pests.
CN202210010159.6A 2022-01-06 2022-01-06 Spinosad suspending agent and preparation method and application thereof Pending CN115812721A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101773124A (en) * 2010-02-12 2010-07-14 浙江升华拜克生物股份有限公司 Compound pesticide
CN102113516A (en) * 2010-01-05 2011-07-06 海南正业中农高科股份有限公司 Insect killing compound containing chlorantraniliprole

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102113516A (en) * 2010-01-05 2011-07-06 海南正业中农高科股份有限公司 Insect killing compound containing chlorantraniliprole
CN101773124A (en) * 2010-02-12 2010-07-14 浙江升华拜克生物股份有限公司 Compound pesticide

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