CN109511671A - Pesticide dinotefuran aqua and its preparation method - Google Patents
Pesticide dinotefuran aqua and its preparation method Download PDFInfo
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- CN109511671A CN109511671A CN201811221186.8A CN201811221186A CN109511671A CN 109511671 A CN109511671 A CN 109511671A CN 201811221186 A CN201811221186 A CN 201811221186A CN 109511671 A CN109511671 A CN 109511671A
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- Prior art keywords
- dinotefuran
- aqua
- pesticide
- emulsifier
- organic solvent
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
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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)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention discloses pesticide dinotefuran aqua, and each component is measured by percentage to the quality: dinotefuran 1-30%, organic solvent 2.5-45%, emulsifier 4-10%, stabilizer 1-3%, antifreezing agent 2-4%, water supply surplus；Organic solvent be selected from one of N-METHYLFORMAMIDE, pyrrolidones, sulfoxide or more than one；Emulsifier is nonionic emulsifier, the 1-3 kind in alkyl phenol polyoxyethylene ether, triphenoethyl benzene phenol polyoxypropylene office ethylene oxide block polymer, phenethyl phenol polyethenoxy ether, special octyl phenol polyoxyethylene ether, oily polyvinylether of combing, alkylphenol-formaldehyde resin polyoxyethylene phenol；Stabilizer selects phosphoric acid aromatic ester or phosphoric acid fatty ester；Antifreezing agent selects ethylene glycol or dimethyl sulfoxide.Dinotefuran aqua provided by the invention, effective component dinotefuran are present in the solution that preparation itself is used with dilution in the form of molecule, ion, and strong to the epidermal permeability and penetrability of pest, the high holding effect of drug effect is long, environmental-friendly.
Description
Technical field
The invention belongs to technical field of agricultural chemical insecticide, in particular to a kind of pesticide dinotefuran aqua and its preparation method.
Background technique
At present China registration the formulations of pesticide containing dinotefuran active ingredients of the original drug have pulvis, granule, suspending agent,
The dosage forms such as missible oil, water dispersible granules, aqueous emulsion, soluble liquid, microemulsion.The pesticidal preparations such as many dinotefuran dosage forms are appealed,
Being watered into liquid particle when emulsion is applied when in use is all micron (um) grade or nanometer (nm) grade.Why without furan
Worm aqueous amine agent is because existing pesticide combination technology is difficult to solve the problems, such as the physical and chemical stability that dinotefuran is made into aqua.
Dinotefuran aqua dosage form is characterized in that, when either its preparation itself is still diluted with water to using multiple, furan
Worm amine raw medicine be all always in water exist in the form of molecule, ion level, therefore dinotefuran aqua dosage form to polypide epidermis and
The permeability of plant surface is more preferable, is easier that pest is made to be poisoned and be absorbed by plants than micron order or nanoscale, meanwhile, plant
The absorbability insecticidal effect of dinotefuran can be further enhanced after absorption.
Therefore researching and developing efficient one kind, low toxicity, environment amenable dinotefuran aqueous pesticide has particularly significant meaning
Justice.
Summary of the invention
The present invention is intended to provide a kind of dinotefuran active ingredients of the original drug be present in the form of molecule, ion preparation itself and
It dilutes in the solution used, strong to the epidermal permeability and penetrability of pest, the high holding effect of drug effect is long, environmental-friendly pesticide furan worm
Aqueous amine agent and its preparation method.
In order to achieve the above objectives, realization that the present invention adopts the following technical solutions:
A kind of pesticide dinotefuran aqua, including dinotefuran, organic solvent, emulsifier and water, wherein each component is with mass percent
Concentration is metering: dinotefuran 1-30%, organic solvent 2.5-45%, emulsifier 4-10%, stabilizer 1-3%, water supply surplus.
It further, further include antifreezing agent 2-4% in the dinotefuran aqua.
Further, the organic solvent be selected from one of N-METHYLFORMAMIDE, pyrrolidones, sulfoxide or it is a kind of with
On.
Further, the emulsifier selects non-ionic emulsifier.
Further, the nonionic emulsifier is selected from alkyl phenol polyoxyethylene ether, triphenoethyl benzene phenol polyoxypropylene
Office's ethylene oxide block polymer, phenethyl phenol polyethenoxy ether, special octyl phenol polyoxyethylene ether, comb oily polyvinylether, alkyl phenol
1-3 kind in formaldehyde resin polyoxyethylene phenol.
Further, the antifreezing agent selects ethylene glycol or dimethyl sulfoxide.
Further, the stabilizer selects phosphoric acid aromatic ester or phosphoric acid fatty ester.
The present invention also provides the preparation methods of the dinotefuran aqua: according to the mass percent, by dinotefuran elder generation
After being added to reaction kettle, organic solvent, emulsifier, antifreezing agent and stabilizer are sequentially added, is stirred to after being completely dissolved and adds water
Surplus is supplied, finally stirring obtains the dinotefuran aqua of as clear as crystal deposit-free.
The invention has the benefit that dinotefuran active ingredients of the original drug is in the form of molecule, ion in 1. dinotefuran aquas
In the presence of preparation itself in the solution that uses of dilution, it is strong to the epidermal permeability penetrability of pest, and the high holding effect of drug effect is long；
2. replacing a large amount of organic solvent environmental pollutions small, more environmentally friendly with water；
3. replacing a large amount of organic solvents to advantageously reduce product cost with water；
4. replacing the dinotefuran aqua of a large amount of organic solvents nonflammable, non-explosive, not volatile with water, production, storage to product
Deposit, transport, use process it is safer, reduce to application personnel murder by poisoning.
Specific embodiment
For a further understanding of the present invention, it is described in further detail below with reference to the embodiment of the present invention.
Embodiment 1: 1% dinotefuran aqua (being metering with mass fraction) is prepared
According to the mass percent, after dinotefuran is first added to reaction kettle, organic solvent, emulsifier, antifreezing agent are sequentially added
And stabilizer, it is stirred to after being completely dissolved and adds water and supply surplus, finally stirring obtains the furan of as clear as crystal deposit-free
Worm aqueous amine agent.
Embodiment 2: 5% dinotefuran aqua (being metering with mass fraction) is prepared
According to the mass percent, after dinotefuran is first added to reaction kettle, organic solvent, emulsifier, antifreezing agent are sequentially added
And stabilizer, it is stirred to after being completely dissolved and adds water and supply surplus, finally stirring obtains the furan of as clear as crystal deposit-free
Worm aqueous amine agent.
Embodiment 3: 10% dinotefuran aqua (being metering with mass fraction) is prepared
According to the mass percent, after dinotefuran is first added to reaction kettle, organic solvent, emulsifier, antifreezing agent are sequentially added
And stabilizer, it is stirred to after being completely dissolved and adds water and supply surplus, finally stirring obtains the furan of as clear as crystal deposit-free
Worm aqueous amine agent.
Embodiment 4: 15% dinotefuran aqua (being metering with mass fraction) is prepared
According to the mass percent, after dinotefuran is first added to reaction kettle, organic solvent, emulsifier and stabilization are sequentially added
Agent is stirred to after being completely dissolved and adds water and supply surplus, and finally stirring obtains the dinotefuran water of as clear as crystal deposit-free
Agent.
Embodiment 5: 20% dinotefuran aqua (being metering with mass fraction) is prepared
| Dinotefuran | 20% | |
| Organic solvent | N-Methyl pyrrolidone | 45% |
| Emulsifier | Alkyl phenol polyoxyethylene ether: triphenoethyl benzene phenol polyoxyethylene polyoxypropylene block polymer: special octyl phenol polyoxyethylene ether=1:1:3 | 10% |
| Antifreezing agent | Ethylene glycol | 4% |
| Stabilizer | Phosphorous triphenyl phosphate acid | 1% |
| Water | Complement to 100% |
According to the mass percent, after dinotefuran is first added to reaction kettle, organic solvent, emulsifier, antifreezing agent are sequentially added
And stabilizer, it is stirred to after being completely dissolved and adds water and supply surplus, finally stirring obtains the furan of as clear as crystal deposit-free
Worm aqueous amine agent.
Embodiment 6: 30% dinotefuran aqua (being metering with mass fraction) is prepared
| Dinotefuran | 30% | |
| Organic solvent | Dimethyl sulfoxide | 45% |
| Emulsifier | Alkyl phenol polyoxyethylene ether | 10% |
| Antifreezing agent | 0% | |
| Stabilizer | Triphenyl phosphite | 1% |
| Water | Complement to 100% |
According to the mass percent, after dinotefuran is first added to reaction kettle, organic solvent, emulsifier and stabilization are sequentially added
Agent is stirred to after being completely dissolved and adds water and supply surplus, and finally stirring obtains the dinotefuran water of as clear as crystal deposit-free
Agent.
Embodiment 7: physicochemical property measurement
The dinotefuran aqua of Example 1-6 preparation carries out physicochemical property test, as a result as follows:
Appearance: clear
Transparency temperature region: -5 DEG C -54 DEG C
Low-temperature stability: qualified
Heat storage stability: qualified
Ageing stability: qualified
Embodiment 8:20% dinotefuran aqua and 20% dinotefuran soluble particles agent prevent and treat rice hoppers field control effectiveness test
Planthopper is the important migratory pest of one kind in China's Rice Production.The area that insect pest occurs in recent years is big, range
Extensively seriously threaten the production of rice.Effectively to control causing harm for planthopper, Jiangxi Bo Bang Bioceuticals Inc., which increases, is thrown
Enter to have developed 1-30% dinotefuran aqua and carried out multiple field control effectiveness test, achieves relatively good result.
1. materials and methods
1.1 test medicine
20% dinotefuran soluble particles agent, the production of Mitsui chemistry ACRO Co., Ltd..20% dinotefuran aqua of embodiment 5,
Jiangxi Bo Bang Bioceuticals Inc. sample.
1.2 experimental design
Test totally 2 processing, 4 repetitions, 8 cells.Each plot area 20m2.Minizone and experimental plot surrounding set protection
Row.
It tests and is carried out 1 to 20 June in 2018 in early rice field.Rice varieties are the excellent 957# of Y third.Experimental plot irrigation and drainage are good
Good, fertility is preferable.Each cell management is consistent, and growth period duration of rice is the heading poplar bloassom phase when application.The breeding time of forth generation planthopper
For the low instar nymphs hatching peak phase.Application -18 type knapsack hand sprayer of T agriculture.Operating pressure 0.2-0.3MP0Spray orifice mouth
Diameter 1mm, reagent is fine on June on the same day 2, and 2-3 grades of south wind, 32.8 DEG C of mean daily temperature, relative temperature 80%, 7d mean temperature after medicine
Minimum 27 DEG C, 35 DEG C of highest, relative humidity 72-80%, occur during entire test without the other factors for influencing test effect.
One reagent agent experimental design of table (20 ㎡ of spraying area)
| Processing number | Medicament title | It is administered dosage (g) | Effective ingredient amount (g/hm2) |
| A | 20% dinotefuran soluble particles agent | 9 | 90 |
| B | 20% dinotefuran aqua | 9 | 90 |
2. efficacy survey
2.1 control time
1,3,7,14 d respectively investigate primary residual worm amount after carrying out radix investigation (rejecting long wing adult) medicine before application, with base before medicine
Number relatively calculates Revision insect recluced rate and compares calculating Rectifying efficacies.
2.2 investigation method
Every cell looks into 5 points, and every 2 clumps of rice clap method investigation nymph quantity with basin and reject long wing adult.
2.3 drug effect calculation methods, calculation formula are as follows:
Revision insect recluced rate (%)=(PT0-PT1)/PT0*100
Wherein: borer population living before PT0- application, borer population living after PT1 application
Preventive effect (%)=(PT-CK)/(100-CK) * 100
Wherein: the applying area PT- insect population decreases rate, and the check plot CK- insect population decreases rate.
3. pharmacodynamic results
3.1 influence crop
Test medicine is within the range of experimental dose to rice without any adverse effect.No phytotoxicity generates, and to other non-target lifes
Object is without influence.
3.2 experimental results and analysis
A, the average preventive effect of 1d investigation is respectively after two processing medicines of B: 40.50%, 51.37%；3d investigates average preventive effect difference after medicine
It is: 61.24%, 80%；7d, which investigates average preventive effect, after medicine is respectively: 82.4%, 90.10%；14d investigates average preventive effect difference after medicine
It is: 92.50%, 96.05%.
It can be seen that being above 20% dinotefuran soluble granule for 20% dinotefuran aqua 1 of examination, 3,7,14d preventive effect.
Embodiment 9:20% dinotefuran aqua and 20% dinotefuran suspending agent prevent and treat rice rice lice field control effectiveness test
1. materials and methods
1.1 test medicine
20% dinotefuran suspending agent (sc), the production of Anhui Jia Lian Biotechnology Co., Ltd.20% dinotefuran aqua of embodiment 5
(AS), Jiangxi Bo Bang Bioceuticals Inc. sample.
1.2 experimental design
Test totally 5 processing, 4 repetitions, totally 20 cells.Each 20 ㎡ of plot area.Minizone and experimental plot surrounding set guarantor
Shield row.Dosage is watered 50L per acre.It tests and is carried out 5 to 25 June in 2018 in rice field.Rice varieties are the excellent China of dream two
It accounts for.Experimental plot irrigation and drainage are good, and fertility is preferable.Each cell management is consistent, and growth period duration of rice is the heading poplar bloassom phase when application.Forth generation
The breeding time of planthopper is the low instar nymphs hatching peak phase.Application -18 type knapsack hand sprayer of T agriculture.Operating pressure
0.2-0.3pa.Spray orifice bore 1mm, reagent is fine on June on the same day 8, and 2-3 grades of south wind, 33.5 DEG C of mean daily temperature, relative humidity
80%, minimum 35 DEG C of 28 DEG C of highests of 7d mean temperature, relative humidity 72-80% after medicine, without influencing test effect during entire test
The other factors of fruit occur.
2. efficacy survey
2.1 control time
Insect population investigation (rejecting long wing adult) is carried out before application, 3d, 7d, 14d respectively investigate primary residual worm amount after medicine, with
Radix compares calculating insect population and gradually moves back rate and compare calculating Rectifying efficacies before medicine.
2.2 investigation method
Every cell looks into 5 points, every 2 clumps of rice.Method investigation nymph quantity is clapped with disk and rejects long wing adult.
2.3 drug effect calculation method formula are the same as embodiment 8.
3. pharmacodynamic results
3.1 influence with embodiment 8 crop.
3.2 experimental results and analysis
2 20% dinotefuran aqua of table and 20% dinotefuran suspending agent control efficiency
Data in table 2 are 4 duplicate average values
From table 2 it is known that after 30g/667 ㎡ medication, 20% dinotefuran SC and 20% dinotefuran AS, 3d, 7d, 14d investigation are average anti-
It controls effect and is respectively as follows: 75.33% and 80.00%；80.80% and 83.70%；84.56% and 86.50%.
After 40g/667 ㎡ medication, 20% dinotefuran SC and 20% dinotefuran AS, 3d, 7d, 14d investigate average control efficiency point
Not are as follows: 80.34% and 90.50%；84.78% and 95.60%；88.21% and 99.00%.
It can be seen that 20% dinotefuran aqua (AS) 3d, 7d, 14d control efficiency is averagely higher than 20% dinotefuran suspending agent (SC).
Claims (10)
1. a kind of pesticide dinotefuran aqua, it is characterised in that: including dinotefuran, organic solvent, emulsifier and water, wherein each group
Dividing with mass percent concentration is to measure: dinotefuran 1-30%, organic solvent 2.5-45%, emulsifier 4-10%, stabilizer 1-3%,
Water supplies surplus.
2. pesticide dinotefuran aqua according to claim 1, it is characterised in that: the dinotefuran 18-30%, it is described organic
Solvent 40-45%.
3. pesticide dinotefuran aqua according to claim 1, it is characterised in that: further include antifreeze in the dinotefuran aqua
Agent 2-4%.
4. pesticide dinotefuran aqua according to claim 1, it is characterised in that: the organic solvent is selected from N- methyl formyl
One of amine, pyrrolidones, sulfoxide or more than one.
5. pesticide dinotefuran aqua according to claim 4, it is characterised in that: the pyrrolidones is N- crassitude
Ketone.
6. pesticide dinotefuran aqua according to claim 4, it is characterised in that: the sulfoxide is dimethyl sulfoxide.
7. pesticide dinotefuran aqua according to claim 1, it is characterised in that: the emulsifier selects non-ionic emulsification
Agent, it is poly- that the nonionic emulsifier is selected from alkyl phenol polyoxyethylene ether, triphenoethyl benzene phenol polyoxypropylene office's ethylene oxide block
Close object, phenethyl phenol polyethenoxy ether, special octyl phenol polyoxyethylene ether, comb oily polyvinylether, alkylphenol-formaldehyde resin polyoxy second
1-3 kind in alkene phenol.
8. pesticide dinotefuran aqua according to claim 1, it is characterised in that: the stabilizer selects phosphoric acid aromatic ester or phosphorus
Sour fatty ester.
9. pesticide dinotefuran aqua according to claim 8, it is characterised in that: the phosphoric acid aromatic ester is phosphorous triphenyl phosphate
Ester.
10. pesticide dinotefuran aqua according to claim 1, it is characterised in that: the antifreezing agent selects ethylene glycol or two
Methyl sulfoxide.
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ID=65770996
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6566392B1 (en) * | 2001-09-14 | 2003-05-20 | Sumitomo Chemical Company, Limited | Solid formulation |
| CN102415405A (en) * | 2011-10-31 | 2012-04-18 | 联保作物科技有限公司 | Dinotefuran micron-emulsion and preparation method thereof |
| CN104542681A (en) * | 2014-12-31 | 2015-04-29 | 海利尔药业集团股份有限公司 | Nematicidal compound containing fluensulfone and dinotefuran |
| CN105532656A (en) * | 2016-01-28 | 2016-05-04 | 南京善思生物科技有限公司 | Environment-friendly dinotefuran microemulsion and preparation method thereof |
| CN105638650A (en) * | 2016-01-28 | 2016-06-08 | 南京善思生物科技有限公司 | Environment-friendly dinotefuran microemulsion free of organic solvent and preparation method thereof |
| CN106342873A (en) * | 2016-08-31 | 2017-01-25 | 郭正 | Pesticide containing dinotefuran and ethiofencarb |
| WO2018079565A1 (en) * | 2016-10-25 | 2018-05-03 | 三井化学アグロ株式会社 | Pesticide liquid formulation |
-
2018
- 2018-10-19 CN CN201811221186.8A patent/CN109511671A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6566392B1 (en) * | 2001-09-14 | 2003-05-20 | Sumitomo Chemical Company, Limited | Solid formulation |
| CN102415405A (en) * | 2011-10-31 | 2012-04-18 | 联保作物科技有限公司 | Dinotefuran micron-emulsion and preparation method thereof |
| CN104542681A (en) * | 2014-12-31 | 2015-04-29 | 海利尔药业集团股份有限公司 | Nematicidal compound containing fluensulfone and dinotefuran |
| CN105532656A (en) * | 2016-01-28 | 2016-05-04 | 南京善思生物科技有限公司 | Environment-friendly dinotefuran microemulsion and preparation method thereof |
| CN105638650A (en) * | 2016-01-28 | 2016-06-08 | 南京善思生物科技有限公司 | Environment-friendly dinotefuran microemulsion free of organic solvent and preparation method thereof |
| CN106342873A (en) * | 2016-08-31 | 2017-01-25 | 郭正 | Pesticide containing dinotefuran and ethiofencarb |
| WO2018079565A1 (en) * | 2016-10-25 | 2018-05-03 | 三井化学アグロ株式会社 | Pesticide liquid formulation |
Non-Patent Citations (2)
| Title |
|---|
| 华乃震: "水基性透明液体剂型的加工、性能和差异（I）", 《世界农药》 * |
| 华乃震: "水基性透明液体剂型的加工、性能和差异（II）", 《世界农药》 * |
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