CN105831135A - Fluorine azole activated ester microcapsule suspending agent - Google Patents
Fluorine azole activated ester microcapsule suspending agent Download PDFInfo
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- CN105831135A CN105831135A CN201510020918.7A CN201510020918A CN105831135A CN 105831135 A CN105831135 A CN 105831135A CN 201510020918 A CN201510020918 A CN 201510020918A CN 105831135 A CN105831135 A CN 105831135A
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- suspending agent
- fluorine azoles
- azoles acibenzolar
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Abstract
The invention relates to a fluorine azole activated ester microcapsule suspending agent, which is prepared from the following raw materials by weight: 1-30% of fluorine azole activated ester, 1-30% of a solvent, 0.2-5% of a capsule wall material, 2-5% of an emulsifier, 2-5% of a dispersion agent, 1-10% of an auxiliary agent, and the balance water. Compared with the prior art, the microcapsule suspending agent provided by the invention can improve the duration, reduce the application frequency and improve the farming efficiency.
Description
Technical field
The invention belongs to formulations of pesticide manufacture field, especially relate to a kind of fluorine azoles Acibenzolar microcapsule suspending agent,
With fluorine azoles Acibenzolar as capsule-core, with polyurethane resin as softgel shell.
Background technology
Fluorine azoles Acibenzolar is a kind of plant induced resistance agent, after being applied to crop with extremely low consumption, can improve crop
Resistance against diseases, this compound can be used in mixed way with multiple disinfectant use in agriculture, can improve the preventing and treating of antibacterial
Effect, reduces usage amount, and application prospect is the most wide.
Fluorine azoles Acibenzolar is made conventional pesticide dosage form such as cream, wettable powder, suspending agent, water-dispersible grain
Agent etc., the lasting period is short, if after making microcapsule suspending agent, can extend the lasting period, but not yet has phase at present
The report closed.
Chinese patent CN103704229A discloses the bactericidal composition of a kind of fluorine-containing azoles Acibenzolar, containing living
Property composition A and active component B bactericidal composition, active components A is selected from fluorine azoles Acibenzolar, and activity becomes
Divide B selected from any one compound following: carbendazim, thiophanate-methyl, Prochloraz or its salt, fluorine bacterium azoles,
And the weight ratio of active components A and active component B is 1: 80～60: 1.And said composition makes wettable
Property powder, water dispersible granules, suspending agent, aqueous emulsion, microemulsion, suspension emulsion, microcapsule suspending agent, microcapsule
Suspension-suspending agent.Although this patent is mentioned the microcapsule suspending agent of fluorine azoles Acibenzolar, but, which kind of is using
In this problem of cyst material, proposition isocyanates and polyamine both cyst material monomers be not anti-
Polyureas cyst wall should be formed, more there is no instantiation, itself be unclear, more there is no the technology such as envelop rate
Index, and the support of efficacy data, it is impossible to obtain preparing the microcapsule suspending agent with preferable performance
Technology enlightenment.
Summary of the invention
Defect that the purpose of the present invention is contemplated to overcome above-mentioned prior art to exist and provide a kind of and can improve
Lasting period, reduce spraying times, improve the fluorine azoles Acibenzolar microcapsule suspending agent of farming efficiency.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of fluorine azoles Acibenzolar microcapsule suspending agent, is prepared by the raw material of following weight percent content:
Surplus is water.
Described fluorine azoles Acibenzolar is phendioxin, 2,3-thiadiazoles-7-methanoic acid trifluoro ethyl esters.
The preferred 5-20% of content of fluorine azoles Acibenzolar.
The preferred 5-25% of consumption of solvent, selected from dimethylbenzene, aromatic solvent naphtha, Ketohexamethylene, dimethyl sulfoxide,
One or more in vegetable oil, mineral oil or N-Methyl pyrrolidone.
Cyst material is the carbamide resin that isocyanates is prepared by interface polymerization reaction with polyamine, wherein,
Isocyanates is selected from toluene di-isocyanate(TDI), isophorone diisocyanate or many phenylmethanes polyisocyanates
In one or more, consumption 0.1-3.5%, polyamine be selected from ethylenediamine or hexamethylene diamine, consumption 0.1-1.5%.
The preferred 3-4% of emulsifier, selected from alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether, dehydration
One or more in sorbitol polyoxyethylene ether fatty acid ester or polyoxyethylene polyoxypropylene block copolymer,
Preferably polyoxyethylene polyoxypropylene block copolymer.
The preferred 2-4% of dispersant dosage, selected from sodium lignin sulfonate, naphthalene sulfonate formaldehyde polymer or triphen second
Alkenyl benzene phenol polyethenoxy ether and derivant thereof, preferably tristyrylphenol polyoxyethylene ether.
The preferred 3-7% of adjuvant consumption, selected from antifreeze, viscosity modifier, PH regulator, preservative or
One or more in defoamer.
Use microencapsulation, fluorine azoles Acibenzolar and oil-soluble cyst material are dissolved in a certain amount of solvent
In, then by the effect of emulsifying agent, uniformly it is emulsifiable in water under high speed shear, oil-soluble monomer and water
Soluble monomers passes through interface polymerization reaction, forms the capsule with polyureas as cyst wall, a diameter of 1-10 of this medicine-carrying capsule
Micron, under the effect of dispersant, even suspension is in water, forms microcapsule suspending agent.
Compared with prior art, the present invention can improve the lasting period, reduces spraying times, improves farming efficiency,
The fluorine azoles Acibenzolar microcapsule suspending agent that cyst material used by the present invention is made, has the highest envelop rate, lives
Property composition got up by effectively cladding, it is to avoid active component is applied to the loss behind field, has thereby served to carry
The effect of high lasting period.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1:
5% fluorine azoles Acibenzolar microcapsule suspending agent
The fluorine former medicine of azoles Acibenzolar (phendioxin, 2,3-thiadiazoles-7-methanoic acid trifluoro ethyl esters) and solvent are added thermosol
Solve uniformly, and add isocyanates and stir, for oil phase, by polyoxyethylene polyoxypropylene block polymer,
Ethylene glycol, sodium benzoate and deionized water are stirred for aqueous phase, then under high-shear emulsifying, oil phase is fast
Speed adds in aqueous phase, adjusts shear rate and makes mean diameter reach 7 microns, then the feed liquid that emulsifying is good is added
Enter in 200ml four-hole boiling flask, then drip ethylenediamine, little in 30 DEG C of insulations 10 under medium mixing speed
Time, it is eventually adding xanthan gum modulation uniformly, i.e. obtains 5% fluorine azoles Acibenzolar microcapsule suspending agent.
Embodiment 2:
10% fluorine azoles Acibenzolar microcapsule suspending agent
The fluorine former medicine of azoles Acibenzolar (phendioxin, 2,3-thiadiazoles-7-methanoic acid trifluoro ethyl esters) and solvent are added thermosol
Solve uniformly, and add isocyanates and stir, for oil phase, by polyoxyethylene polyoxypropylene block polymer,
Ethylene glycol, sodium lignin sulfonate, sodium benzoate and deionized water are stirred for aqueous phase, then in high shear
Under emulsifying, oil phase is rapidly joined in aqueous phase, adjust shear rate and make mean diameter reach 5 microns, then will
The good feed liquid of emulsifying adds in 200ml four-hole boiling flask, then drips ethylenediamine, under medium mixing speed in
30 DEG C are incubated 10 hours, are eventually adding xanthan gum modulation uniformly, i.e. obtain 10% fluorine azoles Acibenzolar microcapsule and hang
Floating agent.
Embodiment 3:
20% fluorine azoles Acibenzolar microcapsule suspending agent
The fluorine former medicine of azoles Acibenzolar (phendioxin, 2,3-thiadiazoles-7-methanoic acid trifluoro ethyl esters) and solvent are added thermosol
Solve uniformly, and add isocyanates and stir, for oil phase, by polyoxyethylene polyoxypropylene block polymer,
Ethylene glycol, sodium benzoate and deionized water are stirred for aqueous phase, then under high-shear emulsifying, oil phase is fast
Speed adds in aqueous phase, adjusts shear rate and makes mean diameter reach 5 microns, then the feed liquid that emulsifying is good is added
Enter in 200ml four-hole boiling flask, then drip ethylenediamine, little in 30 DEG C of insulations 10 under medium mixing speed
Time, it is eventually adding xanthan gum modulation uniformly, i.e. obtains 20% fluorine azoles Acibenzolar microcapsule suspending agent.
The key technical indexes of the present invention is as follows:
Fluorine azoles Acibenzolar microcapsule suspending agent of the present invention can be used for Semen Tritici aestivi, Oryza sativa L., Cotton Gossypii, Semen arachidis hypogaeae, vegetables
Dish, fruit tree, Nicotiana tabacum L., flowers, ornamental plant and lawn etc., for prevention and control ascomycetes, basidiomycetes, partly know
Powdery mildew that bacterium and Oomycete fungal cause, downy mildew, leaf mold, melasma, epidemic disease, rust, anthrax
The multiple diseases such as disease, root rot, damping-off, damping off, verticillium wilt, to part bacterial disease such as scab
Disease, bacterial wilt, Peptic Ulcers etc. have certain induced resistance.Additionally, fluorine azoles Acibenzolar microcapsule suspending agent is to little
Diamond-back moth has certain anti-insect activity concurrently.
Select fluorine azoles Acibenzolar microcapsule suspending agent product and other dosage forms of identical effective ingredient in embodiment respectively
Carry out cucumber downy mildew, Citrullus vulgaris powdery mildew, leaf muld of tomato and the preventing and treating of watermelon blight.
Reference examples:
Contrast test with fluorine azoles Acibenzolar cream
1. test material
Reagent agent: 5%, 10%, 20% fluorine azoles Acibenzolar microcapsule suspending agent；Comparison medicament: 5% fluorine azoles
Acibenzolar cream.Above medicament is provided by Taihe Chemical Industry Co. Ltd., Shanghai.
For examination object: cucumber downy mildew (Pseudoperonospora cubensis), Citrullus vulgaris powdery mildew
(Sphaerotheca cucurbitae), leaf muld of tomato (Cladosporium fulvum), Citrullus vulgaris are withered
Sick (Fusarium oxysporum)
2. test method
Use pot-culture method, in Fructus Cucumidis sativi two leaf one heart stage, Citrullus vulgaris two leaf one heart stage, the Fructus Lycopersici esculenti four leaf phase the
Dispenser, fluorine azoles Acibenzolar uses foliar spray mode dispenser, uniformly sprays application to the positive back side of blade, execute
Concentration 20mg/L, is advisable with blade face droplet uniformity, induces 1 time every 7d, continuous induction 3 times,
3d inoculation after 3rd induction.Cucumber downy mildew, Citrullus vulgaris powdery mildew and leaf muld of tomato all use blade face to spray
Mist method is inoculated, and watermelon blight uses pouring root mode to inoculate.The investigation state of an illness when clear water comparison morbidity is uniform
And calculating prevention effect.
3. investigation method
Cucumber downy mildew, Citrullus vulgaris powdery mildew, leaf muld of tomato calculate preventive effect according to the grade scale investigation state of an illness；
Watermelon blight investigation diseased plant number, adds up diseased plant rate.
Downy mildew, powdery mildew and leaf mold disease leaf grade scale (ginseng GB/T 17980.54～17980.148-2004
With GB/T 17980.1～17980.53-2000).
4. result and analysis
Take 3 fluorine azoles Acibenzolar microcapsule suspension agent prescriptions in the embodiment of the present invention, with 5% fluorine azoles Acibenzolar breast
Oil carries out contrast test for doing comparison, and fluorine azoles Acibenzolar spraying medicine concentration is 20mg/L, and each process sets 3 weights
Multiple, result takes 3 meansigma methodss repeated.7 days the most after administration, 14 days and 21 days investigation medicaments pair
The induction disease resisting effect of cucumber downy mildew, Citrullus vulgaris powdery mildew, leaf muld of tomato and watermelon blight.
(1) the induction disease resisting effect to cucumber downy mildew
After dispenser 7 days, invention formulation and fluorine azoles Acibenzolar cream drug effect aspect there was no significant difference, but with
Time lengthening, after medicine after 14 days and medicine 21 days, fluorine azoles Acibenzolar microcapsule suspending agent of the present invention was to Fructus Cucumidis sativi
Downy mildew still maintains higher preventive effect, wherein embodiment 1 and embodiment 2 fluorine azoles Acibenzolar microcapsule suspending agent
After medicine, the preventive effect of 21 days is still more than 70%, and being decreased obviously occurs in the preventive effect of fluorine azoles Acibenzolar cream,
Preventive effect is only 63.67% (table 1).
Table 1 fluorine azoles Acibenzolar (FBT) microcapsule suspending agent induction disease resisting effect to cucumber downy mildew
(2) the induction disease resisting effect to Citrullus vulgaris powdery mildew
After dispenser 7 days, invention formulation and fluorine azoles Acibenzolar cream drug effect aspect there was no significant difference, but with
Time lengthening, after medicine 21 days, Example 1 and Example 2 of the present invention fluorine azoles Acibenzolar microcapsule suspension
Agent still maintains higher preventive effect to Citrullus vulgaris powdery mildew, and preventive effect is respectively 75.03% and 71.71%, and cream
But occur that significance declines, show that Citrullus vulgaris powdery mildew is had longer compared with cream by fluorine azoles Acibenzolar microcapsule suspending agent
Lasting effect.
Table 2 fluorine azoles Acibenzolar (FBT) microcapsule suspending agent induction disease resisting effect to Citrullus vulgaris powdery mildew
(3) the induction disease resisting effect to leaf muld of tomato
After dispenser 7 days, invention formulation and fluorine azoles Acibenzolar cream drug effect aspect there was no significant difference, but with
Time lengthening, after medicine after 14 days and medicine 21 days, fluorine azoles Acibenzolar microcapsule suspending agent of the present invention three was joined
The square induction preventive effect to leaf muld of tomato is all more than 70%, and cream occurs that significance declines
(66.19%), show that fluorine azoles Acibenzolar microcapsule suspending agent has longer holding effect compared with cream to leaf muld of tomato
Property.
Table 3 fluorine azoles Acibenzolar (FBT) microcapsule suspending agent induction disease resisting effect to leaf muld of tomato
(4) the induction disease resisting effect to cucumber fusarium axysporum
After dispenser 7 days, invention formulation and fluorine azoles Acibenzolar cream drug effect aspect there was no significant difference, but with
Time lengthening, after medicine after 14 days and medicine 21 days, Example 1 and Example 2 of the present invention fluorine azoles activated
Ester micro capsule suspending agent still maintains higher preventive effect to cucumber fusarium axysporum, and cream occurs that significance declines,
Show that fluorine azoles Acibenzolar microcapsule suspending agent has longer lasting effect compared with cream to cucumber fusarium axysporum.
Table 4 fluorine azoles Acibenzolar (FBT) microcapsule suspending agent induction disease resisting effect to cucumber fusarium axysporum
Embodiment 4
A kind of fluorine azoles Acibenzolar microcapsule suspending agent, is prepared by the raw material of following weight percent content: fluorine
Azoles Acibenzolar 1%, solvent 1%, cyst material 0.2%, emulsifying agent 2%, dispersant 2%, adjuvant 1%,
Surplus is water.Wherein, fluorine azoles Acibenzolar is phendioxin, 2,3-thiadiazoles-7-methanoic acid trifluoro ethyl esters, and solvent selects
With Ketohexamethylene, cyst material is the carbamide resin that isocyanates is prepared by interface polymerization reaction with polyamine,
Wherein, isocyanates is isophorone diisocyanate, and consumption is 0.1%, and polyamine is ethylenediamine, consumption
Being 0.1%, emulsifying agent is polyoxyethylene polyoxypropylene block copolymer, and dispersant is that triphenyl vinyl phenol gathers
Oxygen vinyl Ether, adjuvant can select antifreeze, viscosity modifier, PH regulator, preservative or froth breaking
One or more in agent.
Use microencapsulation, fluorine azoles Acibenzolar and oil-soluble cyst material are dissolved in a certain amount of solvent
In, then by the effect of emulsifying agent, uniformly it is emulsifiable in water under high speed shear, oil-soluble monomer and water
Soluble monomers passes through interface polymerization reaction, forms the capsule with polyureas as cyst wall, a diameter of 1-10 of this medicine-carrying capsule
Micron, under the effect of dispersant agent, even suspension is in water, forms microcapsule suspending agent, below concrete employing
Step:
Step 1, the fluorine former medicine of azoles Acibenzolar is dissolved in appropriate solvent, adds appropriate isocyanates cyst wall
Material monomer, stirs, as oil phase；
Step 2, emulsifying agent, defoamer, antifreezing agent, preservative are added in suitable quantity of water, stir,
As aqueous phase；
Step 3, oil phase is made an addition to aqueous phase, stir or by high-shear emulsifying, until mean diameter reaches
To 1-10 micron；
Step 4, by feed liquid good for emulsifying 20-70 DEG C of insulated and stirred, and adding polyamine, to participate in polymerization anti-
Should, the encystation time is 2-10 hour；
The auxiliary agents such as step 5, addition viscosity modifier, stir and i.e. make fluorine azoles Acibenzolar microcapsule suspension
Agent.
Embodiment 5
A kind of fluorine azoles Acibenzolar microcapsule suspending agent, is prepared by the raw material of following weight percent content: fluorine
Azoles Acibenzolar 5%, solvent 5%, cyst material 3%, emulsifying agent 3%, dispersant 2%, adjuvant 3%,
Surplus is water.Fluorine azoles Acibenzolar is phendioxin, 2,3-thiadiazoles-7-methanoic acid trifluoro ethyl esters, and solvent is dimethyl
Sulfoxide and the mixture of N-Methyl pyrrolidone.Cyst material is that isocyanates passes through interfacial polymerization with polyamine
The carbamide resin that reaction prepares, wherein, isocyanates is many phenylmethanes polyisocyanates, and consumption is 2.0%
Polyamine is hexamethylene diamine, and consumption is 1.0%.Emulsifying agent is alkylphenol polyoxyethylene and aliphatic alcohol polyethenoxy
The mixture of ether.Dispersant is naphthalene sulfonate formaldehyde polymer.Adjuvant can be selected from antifreeze, viscosity is adjusted
One or more in joint agent, PH regulator, preservative or defoamer, its preparation method and embodiment 4
Identical.
Embodiment 6
A kind of fluorine azoles Acibenzolar microcapsule suspending agent, is prepared by the raw material of following weight percent content: fluorine
Azoles Acibenzolar 25%, solvent 25%, cyst material 4%, emulsifying agent 4%, dispersant 4%, adjuvant
7%, surplus is water.Fluorine azoles Acibenzolar is phendioxin, 2,3-thiadiazoles-7-methanoic acid trifluoro ethyl esters.Solvent is
Vegetable oil, cyst material is the carbamide resin that isocyanates is prepared by interface polymerization reaction with polyamine, its
In, isocyanates is many phenylmethanes polyisocyanates, and consumption is 3.5%, and polyamine is ethylenediamine, consumption
Being 0.5%, emulsifying agent is anhydrous sorbitol polyoxyethylene ether fatty ester.Dispersant is sodium lignin sulfonate,
Adjuvant one or several in antifreeze, viscosity modifier, PH regulator, preservative or defoamer
Kind, its preparation method is the same as in Example 4.
Embodiment 7
A kind of fluorine azoles Acibenzolar microcapsule suspending agent, is prepared by the raw material of following weight percent content: fluorine
Azoles Acibenzolar 30%, solvent 30%, cyst material 5%, emulsifying agent 5%, dispersant 5%, adjuvant 10%,
Surplus is water.Fluorine azoles Acibenzolar is phendioxin, 2,3-thiadiazoles-7-methanoic acid trifluoro ethyl esters.Solvent is mineral oil,
Cyst material is the carbamide resin that isocyanates is prepared by interface polymerization reaction with polyamine, and isocyanates is
Toluene di-isocyanate(TDI), consumption is 3.5%, and polyamine is hexamethylene diamine, and consumption is 1.5%.Emulsifying agent is alkane
Base phenol polyethenoxy ether, dispersant is naphthalene sulfonate formaldehyde polymer, and adjuvant can be selected from antifreeze, glue
One or more in degree regulator, PH regulator, preservative or defoamer, its preparation method and enforcement
Example 4 is identical.
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.Should refer to
Go out, for those skilled in the art, under the premise without departing from the principles of the invention, also
The present invention can be carried out some improvement and modification, these improve and modify and also fall into the claims in the present invention
In protection domain.
Claims (8)
1. a fluorine azoles Acibenzolar microcapsule suspending agent, it is characterised in that this suspending agent is by following weight percent
Prepare than the raw material of content:
A kind of fluorine azoles Acibenzolar microcapsule suspending agent the most according to claim 1, it is characterised in that institute
The fluorine azoles Acibenzolar stated is phendioxin, 2,3-thiadiazoles-7-methanoic acid trifluoro ethyl esters.
A kind of fluorine azoles Acibenzolar microcapsule suspending agent the most according to claim 1, it is characterised in that institute
The preferred 5-20% of content of the fluorine azoles Acibenzolar stated.
A kind of fluorine azoles Acibenzolar microcapsule suspending agent the most according to claim 1, it is characterised in that institute
The preferred 5-25% of consumption of the solvent stated, selected from dimethylbenzene, aromatic solvent naphtha, Ketohexamethylene, dimethyl sulfoxide,
One or more in vegetable oil, mineral oil or N-Methyl pyrrolidone.
A kind of fluorine azoles Acibenzolar microcapsule suspending agent the most according to claim 1, it is characterised in that institute
The cyst material stated is the carbamide resin that isocyanates is prepared by interface polymerization reaction with polyamine,
Described isocyanates is selected from toluene di-isocyanate(TDI), isophorone diisocyanate or many phenylmethanes
One or more in polyisocyanates, consumption 0.1-3.5%；
Described polyamine is selected from ethylenediamine or hexamethylene diamine, consumption 0.1-1.5%.
A kind of fluorine azoles Acibenzolar microcapsule suspending agent the most according to claim 1, it is characterised in that institute
The preferred 3-4% of emulsifier stated, selected from alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether, dehydration
One or more in sorbitol polyoxyethylene ether fatty acid ester or polyoxyethylene polyoxypropylene block copolymer,
Preferably polyoxyethylene polyoxypropylene block copolymer.
A kind of fluorine azoles Acibenzolar microcapsule suspending agent the most according to claim 1, it is characterised in that institute
The preferred 2-4% of dispersant dosage stated, selected from sodium lignin sulfonate, naphthalene sulfonate formaldehyde polymer or triphen second
Alkenyl benzene phenol polyethenoxy ether and derivant thereof, preferably tristyrylphenol polyoxyethylene ether.
A kind of fluorine azoles Acibenzolar microcapsule suspending agent the most according to claim 1, it is characterised in that institute
The preferred 3-7% of adjuvant consumption stated, selected from antifreeze, viscosity modifier, PH regulator, preservative or
One or more in defoamer.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510020918.7A CN105831135A (en) | 2015-01-15 | 2015-01-15 | Fluorine azole activated ester microcapsule suspending agent |
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| CN201510020918.7A CN105831135A (en) | 2015-01-15 | 2015-01-15 | Fluorine azole activated ester microcapsule suspending agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2613807A (en) * | 2021-12-15 | 2023-06-21 | Rotam Agrochem Int Co Ltd | Microcapsule pesticide formulation and the use thereof |
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2015
- 2015-01-15 CN CN201510020918.7A patent/CN105831135A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2613807A (en) * | 2021-12-15 | 2023-06-21 | Rotam Agrochem Int Co Ltd | Microcapsule pesticide formulation and the use thereof |
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Application publication date: 20160810 |