CN103651381B - A kind of mite-killing preparation and application thereof - Google Patents
A kind of mite-killing preparation and application thereof Download PDFInfo
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- CN103651381B CN103651381B CN201210358582.1A CN201210358582A CN103651381B CN 103651381 B CN103651381 B CN 103651381B CN 201210358582 A CN201210358582 A CN 201210358582A CN 103651381 B CN103651381 B CN 103651381B
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Abstract
The invention belongs to agricultural acaricides field, relating to a kind of take compd A as the aqueous suspension agent of acaricidal activity component, and the structural formula of compd A is as follows:
Description
Technical field
The invention belongs to miticide field, relate to a kind of vinyl cyanide miticide preparation, relate to particularly with compound disclosed in CN101875633A 5 be active component a kind of mite-killing preparation and application thereof.
Background technology
As everyone knows, miticide has obvious effect in control agricultural evil mite or urban health evil mite.But miticide is in use for some time, evil mite can produce certain resistance, along with people are to the growing needs such as Pesticidal products and the pay attention to day by day to environmental protection, and low, the environment amenable miticide kind of agriculturally active demand use cost.Disclosed in CN101875633A, compound 5(is hereinafter referred to as compd A) if become the preventive effect of mite mite, the equal tool excellence of mite ovum to evil mite as Tetranychus cinnabarinus, to crop safety, be a kind of efficient miticide, there is wide market application foreground.The structure of compd A is as follows:
Only mention compd A in prior art and can be processed into preparation, but there is no concrete technical scheme.The needs of a kind of class creamy " formulation " just in order to meet biological activity test that CN101875633A adopts matching while using to obtain when testing former medicine biologically active, both do not meet the requirement of Pesticide formulation specified standard, be difficult to the needs meeting practical application yet.But, there is no the report for compd A preparation research at present.
Summary of the invention
The object of the invention is to develop a kind of take compd A as the mite-killing preparation of active component.Because aqueous suspension agent not only has the advantages such as particle diameter is little, good dispersion, good fluidity, suspensibility are high, biologically active is high, using dosage is little, and have resistance of rainwater washing against, residual low, to advantages such as people and animals' low toxicities, drift about without dust in the manufacture and usage of simultaneously aqueous suspension agent, nonflammable explosive, safety good, be easy to packaging, transport and storage, therefore object of the present invention be exploitation a kind of take compd A as the miticide aqueous suspension agent of active component, to meet agricultural production practical application, to play former medicine biologically active, effectively control evil mite better.
In order to realize object of the present invention, inventor, according to its action target and application mode, by screening the suitable auxiliaries mated with active ingredient, determines a kind of miticide aqueous suspension agent formula.This aqueous suspension agent can improve wetting, the spread of active ingredient on crop target, dispersion, delay and permeance property, reaches the object improving its acaricidal activity, reduce use cost, preserve the ecological environment, thus achieves object of the present invention.
Agricultural chemicals itself is that a class has bioactive speciality chemical, and the auxiliary agent of dissimilar, different chemical structures, has considerable influence to the activity of compd A.Same Target crops, uses different surfactants, and its assimilation effect is also not quite similar, the difference in this activity brought by this body structure of surfactant, is difficult to compensate by the way improving concentration.Outstanding feature of the present invention is exactly by selecting and adding the adjuvant system of mating with compd A, this adjuvant system contributes to active ingredient solubilising and has good wetting action to dispersed pesticide activity component particle external surface and porous surface, be adsorbed in the surface of former medicine particle, form the adsorption layer of comparatively dense, make mutually to repel between particle with the interaction of " steric hindrance ", thus make it dispersed, agricultural chemicals particle can also be stoped to assemble once again in adjustment and storage period, it is made to keep a kind of dispersiveness well, appearance stability and heat storage stability, reduce rate of crystalline growth.The dilution of said preparation has higher plate-out ability and adhesivity on control target simultaneously; thus obviously improve wetting, the spread of its liquid, dispersion, delay and permeance property; reduce spray liquor (air-flow) drift with the wind; thus be beneficial to liquid and sprawl on blade face and stick; reach and improve its biologically active; significantly reduce the effective ingredient consumption of agricultural chemicals, reduce costs, the object of preserving the ecological environment.
Auxiliary agent kind selected by aqueous suspension agent of the present invention is good to Environmental compatibility, does not increase former medicine to mammiferous toxicity, does not produce poisoning to crop; Good chemical stability is possessed to pesticide original medicine; Do not reduce the biologically active of pesticide active ingredient; In use can improve the dispersity of active ingredient and active ingredient to the deposition of target body and deposition fraction; Consumption is few, to the strong adaptability of operation technique condition.
Technical scheme of the present invention is as follows:
A kind of miticide aqueous suspension agent is active component with compd A, containing dispersant, antifreezing agent and water in preparation; In described aqueous suspension agent, the weight percentage of each component is: compound A-40 .5 ~ 70%, dispersant 1 ~ 50%, antifreezing agent 1 ~ 20%, water 5 ~ 90%.
The comparatively preferred technical scheme of the present invention is:
In miticide aqueous suspension agent, the weight percentage of each component is: compound A-45 ~ 50%, dispersant 5 ~ 30%, antifreezing agent 1 ~ 10%, water 15 ~ 80%.
Preferred technical scheme is further:
In miticide aqueous suspension agent, the weight percentage of each component is: compd A 10 ~ 30%, dispersant 8 ~ 20%, antifreezing agent 2 ~ 8%, water 45 ~ 80%.
The dispersant kind related in miticide aqueous suspension agent formula of the present invention multi-section about surfactant and the formulations of pesticide processing monograph in all have report.Such as, " surfactant science and application ", the chief editors such as Jiang Qingzhe, Sinopec publishing house, 2009; " special surfactant ", the chief editors such as Wang Peiyi, China Textiles Press; " formulations of pesticide process technology ", Liu Bulin edits, Chemical Industry Press, 1998; SiselyndWood, EncyclopediaofSurfaceActiveAgents, ChemicalPubl., Co., Inc., NewYork, 1964.
Particularly, the dispersant in miticide aqueous suspension agent of the present invention can be selected from: the sodium salt of alkyl naphthalene sulfonic acid condensation polymer, agriculture breast 0201B, agriculture breast 0203B, agriculture breast 100
#, agriculture breast 500
#, Nongru-700
#, agriculture breast BY110, agriculture breast 1601, agriculture breast T-20, agriculture breast S-80, agriculture breast NP-7, agriculture breast NP-8, agriculture breast NP-15, agriculture breast OX-635, agriculture breast OX-662, sodium lignin sulfonate, Nekal BX, detergent LS, calcium lignosulfonate, methyl naphthalene sulfonate formaldehyde condensate, naphthalenesulfonic acid-formaldehyde condensate, methanonaphthalene sodium sulfonate, oleic acid methylaminoethyl sodium sulfonate, alkyl-diethylene glycol ether-sodium sulfonate, N-methyl-oleoyl-sodium taurocholate, dibutyl naphthalenesulfonic acid formaldehyde condensation products, epoxidized polyether, to tertbutyl ether, castor oil ethylene oxide adduct, ethylene oxide-propylene oxide block copolymer, alkylphenol polyoxyethylene formaldehyde condensation products, one or more in alkylphenol-polyethenoxy polyethenoxy ether or methylcellulose.Also can with selecting the PICO series of products of Japanese Zhu Ben's Oil Corporation if PICO-LF1, PICO-LF3, PICO-LF7, PICO-LF1, PICO-LPQ are as dispersant.
Preferred dispersant is further: the sodium salt of alkyl naphthalene sulfonic acid condensation polymer, agriculture breast NP-7, agriculture breast NP-8, agriculture breast NP-15, agriculture breast 0201B, agriculture breast 0203B, Nongru-700
#, agriculture breast BY110, agriculture breast 1601, agriculture breast T-20, agriculture breast S-80, methyl naphthalene sulfonate formaldehyde condensate, naphthalenesulfonic acid-formaldehyde condensate or methanonaphthalene sodium sulfonate in one or more.
Antifreezing agent in miticide aqueous suspension agent of the present invention can be selected from: ethylene glycol, glycerine, propane diols, polyethylene glycol, sorbierite or urea.
Preferred antifreezing agent is ethylene glycol or glycerine further.
In addition, the physical stability that appropriate thickener can improve aqueous suspension agent is added in some cases, as reduced layering, being convenient to packaging.Thickener in miticide aqueous suspension agent of the present invention can be selected from: one or more in xanthans, gelatin, gum Arabic, polyvinyl acetate, polyvinylpyrrolidone, aluminium-magnesium silicate, polyvinyl alcohol, polyethylene glycol, phenolic resins, shellac, CMC, hydroxyethylcellulose, hydroxypropyl cellulose, methylcellulose and sodium alginate.But part dispersant also can have effect of thickener in some cases.
In miticide aqueous suspension agent of the present invention in some cases (when in filling a prescription containing the material such as polysaccharose substance easily gone mouldy time) add the situation of easily going mouldy when a small amount of preservative can improve aqueous suspension agent storage, preservative can be selected from usually: one or more in Sodium Benzoate, Kathon CG (MIT and (B) CMIT), potassium sorbate, dehydro sodium acetate, calcium propionate, sodium Diacetate, sodium lactate, propylparaben.
When preparing aqueous suspension agent, sometimes owing to easily air being brought in plant equipment reason and process, produce bubble, usually need to add appropriate defoamer.Defoamer in miticide aqueous suspension agent of the present invention can be selected from: bubble enemy, silicone oil, silicone, WJX-1, C
8 ~ 10fatty alcohol, C
10 ~ 20saturated fat acids (as capric acid, stearic acid etc.) or C
10 ~ 20unsaturated fatty acid amide.The selection of defoamer is appreciated by those skilled in the art.
The miticide aqueous suspension agent that the present invention relates to adopts conventional method preparation, its compound method is: joined in blending tank with dispersant, antifreezing agent and water ratio on demand by compd A and mix, first through high-speed shearing machine coarse crushing, then be pumped in sand mill and carry out fine grinding, when the average grain diameter of 95% material reaches below 5 μm of particle diameters, filter, miticide aqueous suspension agent product of the present invention can be obtained.
Adopt the aqueous suspension agent containing active constituent compound A of formulated of the present invention, biologically active is excellent, and its acaricidal activity is significantly better than the measurement result preparing former medicine by the method provided in CN101875633A.
Miticide aqueous suspension agent of the present invention before use through diluting or being directly watered spraying, also can directly can use.
Technical scheme of the present invention also comprises the method for control evil mite: imposed on described harmful mite or its somatomedin by miticide aqueous suspension agent of the present invention.The comparatively suitable effective amount of usual selection is per hectare 10 grams to 1000 grams.
Technical scheme of the present invention also comprises the purposes of above-mentioned miticide aqueous suspension agent: for the preparation of the purposes of killing mite aqueous suspension agent medicine, miticide aqueous suspension agent of the present invention can be applicable to the control of Agricultural Mites, forestry harmful mites or non-treatment object health evil mite, if especially become the preventive effect of mite mite, the equal tool excellence of mite ovum, to crop safety to evil mite such as Tetranychus cinnabarinus.
Miticide aqueous suspension agent of the present invention has the following advantages: 1) flash-point is high, nonflammable, explosive, storage, use safety; 2) dust is few, and environmental pollution is little, uses conveniently, to the producer and user and Environmental security; 3) aqueous suspension agent take water as matrix, aboundresources, and product cost is low, easily packs; 4) have particle diameter little, good dispersion, good fluidity, suspensibility are high, biologically active is high, using dosage is little, resistance of rainwater washing against, residual low, to features such as people and animals' low toxicities; 5), after aqueous suspension agent spraying, be distributed in crop surface with fine particle, miticidal effect is good; 6) saving of labor, save time, with rational application mode, minimum drug cost, the object of pest control can be reached.
Embodiment
Following specific embodiment is for further describing the present invention, but the present invention is limited to absolutely not these examples.In formula, percentage and number are all by weight.Active constituent compound A self-control (content 98%), roll over hundred post doses and add, other each raw materials are commercially available product.
Pharmaceutical formulation embodiment
Embodiment 1,10% compd A aqueous suspension agent
Compound method is as follows: joined in blending tank successively by above-mentioned substance and mix, first carry out coarse crushing, homogenize through high shear, then be pumped in sand mill and carry out fine grinding, particles distribution instrument detects the granularity of sand milling material, after particle diameter reaches (by 75 μm of standard screen >=98%) standard-required, filter, 10% compd A aqueous suspension agent can be obtained.Following formulation Example is prepared all in the same way.
Embodiment 1 sample all technical is: pH value 6.3; Suspensibility 93.8%; Pourability: topple over rear residue 3.5%, residue 0.2% after washing; Persistent foamability (after 1min) 30mL; Low-temperature stability is qualified; Heat storage stability (54 ± 2) DEG C/14 days, resolution ratio is 1.0%.
Embodiment 2,10% compd A aqueous suspension agent
Embodiment 2 sample all technical is: pH value 6.5; Suspensibility 96.5%; Pourability: topple over rear residue 3.8%, residue 0.2% after washing; Persistent foamability (after 1min) 25mL; Low-temperature stability is qualified; Heat storage stability (54 ± 2) DEG C/14 days, resolution ratio is 1.1%.
Embodiment 3,20% compd A aqueous suspension agent
Embodiment 3 sample all technical is: pH value 6.6; Suspensibility 95.9%; Pourability: topple over rear residue 3.9%, residue 0.3% after washing; Persistent foamability (after 1min) 30mL; Low-temperature stability is qualified; Heat storage stability (54 ± 2) DEG C/14 days, resolution ratio is 1.3%.
Embodiment 4,20% compd A aqueous suspension agent
Embodiment 4 sample all technical is: pH value 6.2, suspensibility 94.8%, pourability: topple over rear residue 3.6%, residue 0.3% after washing, persistent foamability (after 1min) 28mL, and low-temperature stability is qualified; Heat storage stability (54 ± 2) DEG C/14 days, resolution ratio is 1.5%.
Embodiment 5,30% compd A aqueous suspension agent
Embodiment 5 sample all technical is: pH value 6.6, suspensibility 93.6%, pourability: topple over rear residue 3.8%, residue 0.3% after washing, persistent foamability (after 1min) 31mL, and low-temperature stability is qualified; Heat storage stability (54 ± 2) DEG C/14 days, resolution ratio is 0.8%.
Embodiment 6,30% compd A aqueous suspension agent
Embodiment 6 sample all technical is: pH value 6.3, suspensibility 95.1%, pourability: topple over rear residue 4.0%, residue 0.3% after washing, persistent foamability (after 1min) 27mL, and low-temperature stability is qualified; Heat storage stability (54 ± 2) DEG C/14 days, resolution ratio is 1.2%.
Embodiment 7,30% compd A aqueous suspension agent
Embodiment 7 sample all technical is: pH value 6.8, suspensibility 92.9%, pourability: topple over rear residue 3.5%, residue 0.2% after washing, persistent foamability (after 1min) 20mL, and low-temperature stability is qualified; Heat storage stability (54 ± 2) DEG C/14 days, resolution ratio is 1.0%.
Embodiment 8,30% compd A aqueous suspension agent
Embodiment 8 sample all technical is: pH value 6.5, suspensibility 95.2%, pourability: topple over rear residue 3.2%, residue 0.2% after washing, persistent foamability (after 1min) 22mL, and low-temperature stability is qualified; Heat storage stability (54 ± 2) DEG C/14 days, resolution ratio is 1.1%.
Performance test embodiment
Embodiment 9, stability comparative trial
Mite-killing preparation of the present invention is conventionally mixed with the aqueous suspension agent of desired concn, tests its stability.
With the method provided in CN101875633A preparation compd A in contrast preparation carry out comparative trial.The preparation of control formulation: compd A acetone solution (content of acetone in total solution is no more than 10%), then becomes the solution of desired concn with the Tween 80 solution of 0.1%.
Test result is in table 1.
Table 1. stability comparative test result (normal temperature)
As seen from the above table, control formulation normal temperature is placed after 1 month and can not be used again; And after preparation provided by the invention (aqueous suspension agent prepared with embodiment 5 for embodiment 2, embodiment 4) places 1,6,12 month, surface tension all changes not quite, by the average grain diameter (d of 98%
98) change also little.This shows that aqueous suspension agent of the present invention not only all can meet liquid soaking on target, and As time goes on, levigate particle does not also change substantially.Finer particles, drug effect are better, otherwise, drug effect play poorer.Upper table data confirm the aqueous suspension agent selecting adjuvant system of the present invention to prepare, and use conveniently, are beneficial to the performance of drug effect.
Biological activity test embodiment
Embodiment 10, biologically active comparative trial
The compound method of suspending agent and former medicine is the same.
Test method: the test sample adopting potted plant seedling spray-on process to measure different batches becomes the active size of mite to Tetranychus cinnabarinus.First becoming mite to receive Tetranychus cinnabarinus of the same size is on the Tolerance of Kidney Bean Seedlings blade of first pair of true leaf open and flat phase, after becoming mite stable, count radix; Then by the order even spraying of experimental scheme from low dosage to high dose, every strain 2mL, often processes and repeats for 3 times, separately establish blank.Examination material after process is placed in the observation ward of certain condition, periodic investigation becomes mite number anyway, calculates lethality.
Table 2 section Example formulation samples acaricidal activity measurement result
--*: represent and do not survey.
Claims (4)
1. a mite-killing preparation, is characterized in that: the aqueous suspension agent taking compd A as active component, and in preparation, key component and weight percentage are:
Compd A 10 ~ 30%,
Dispersant 8 ~ 20%,
Antifreezing agent 2 ~ 8%,
Water 45 ~ 80%;
Compound A structure formula is as follows:
Described dispersant be selected from alkyl naphthalene sulfonic acid condensation polymer sodium salt, agriculture breast NP-7, agriculture breast NP-15, agriculture breast 0201B, agriculture breast 0203B, Nongru-700
#, agriculture breast 1601, agriculture breast S-80, methyl naphthalene sulfonate formaldehyde condensate, naphthalenesulfonic acid-formaldehyde condensate or methanonaphthalene sodium sulfonate in one or more;
Described antifreezing agent is selected from ethylene glycol or glycerine.
2. mite-killing preparation according to claim 1, is characterized in that: can also add appropriate thickener, preservative and/or defoamer as required in described aqueous suspension agent.
3. control a method for evil mite, it is characterized in that: mite-killing preparation according to claim 1 is imposed on the harmful mite of needs control or the medium of its growth with 10 ~ 1000 grams of active ingredient/hectares.
4. the purposes of mite-killing preparation as claimed in claim 1 evil mite in control agricultural, forestry or health.
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| CN109221156A (en) * | 2014-12-25 | 2019-01-18 | 沈阳中化农药化工研发有限公司 | Insecticidal and acaricidal composition of the one kind containing fungicide or bactericidal (virus) agent |
| CN106305727B (en) * | 2015-06-18 | 2019-02-15 | 沈阳中化农药化工研发有限公司 | A kind of insecticide acaricide composition containing synergist |
| CN105875659A (en) * | 2016-05-17 | 2016-08-24 | 梁文荣 | Pesticide preparation for killing spider mite |
| CN108684681B (en) * | 2017-03-31 | 2021-03-30 | 沈阳中化农药化工研发有限公司 | Mite killing preparation and application thereof |
| CN108949373A (en) * | 2018-06-29 | 2018-12-07 | 东莞市硕丰研磨科技有限公司 | Glass cleaner |
| CN111789122A (en) * | 2019-04-09 | 2020-10-20 | 浙江省化工研究院有限公司 | A kind of acaricidal composition containing fenpyroxifen and spirocyclic quaternary acid pesticides |
| CN114762502B (en) * | 2021-01-13 | 2023-03-21 | 沈阳中化农药化工研发有限公司 | Acaricide suspending agent and preparation thereof |
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| JP2003201280A (en) * | 2001-10-24 | 2003-07-18 | Nissan Chem Ind Ltd | Acrylonitrile compound |
| JP2003206281A (en) * | 2002-01-10 | 2003-07-22 | Nissan Chem Ind Ltd | Acrylonitrile compound |
| CN101367784B (en) * | 2008-09-28 | 2012-05-30 | 江苏省农药研究所股份有限公司 | Acrylonitrile compound and preparation method and application thereof |
| CN101875633B (en) * | 2009-04-29 | 2012-01-18 | 中国中化股份有限公司 | Pyrazolyl acrylonitrile compound and application thereof |
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