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CN109169733A - A kind of biological agent and preparation method of Control Dendrolimus punctatus - Google Patents

A kind of biological agent and preparation method of Control Dendrolimus punctatus Download PDF

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Publication number
CN109169733A
CN109169733A CN201810890155.5A CN201810890155A CN109169733A CN 109169733 A CN109169733 A CN 109169733A CN 201810890155 A CN201810890155 A CN 201810890155A CN 109169733 A CN109169733 A CN 109169733A
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CN
China
Prior art keywords
biological agent
biomass
parts
dendrolimus punctatus
control
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810890155.5A
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Chinese (zh)
Inventor
张海亮
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Welcome To Yinan County Agricultural Development Co Ltd
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Welcome To Yinan County Agricultural Development Co Ltd
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Priority to CN201810890155.5A priority Critical patent/CN109169733A/en
Publication of CN109169733A publication Critical patent/CN109169733A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/561,2-Diazoles; Hydrogenated 1,2-diazoles
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08Magnoliopsida [dicotyledons]
    • A01N65/34Rosaceae [Rose family], e.g. strawberry, hawthorn, plum, cherry, peach, apricot or almond

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Plant Pathology (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Biotechnology (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Pest Control & Pesticides (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a kind of biological agent of Control Dendrolimus punctatus and preparation methods, belong to biological pesticide technical field.The biological agent is made of active constituent Rynaxypyr, biomass and auxiliary agent.Indoor virulence test proves there is synergistic effect, Small side effects preferable to the control efficiency of pine moth after main ingredient Rynaxypyr and biomass cooperation in biological agent of the present invention.

Description

A kind of biological agent and preparation method of Control Dendrolimus punctatus
Technical field
The invention belongs to the biological agents and preparation of biological pesticide technical field more particularly to a kind of Control Dendrolimus punctatus Method.
Background technique
Masson pine becomes the important reproducting tree species in China because it is with the strong and evergreen characteristic of vitality.Dendrolimus punctatus It is a major pest of masson pine forest, seriously endangers the growth of masson pine forest.It has been found that the process of breaking out of dendrolimus punctatus has Periodical and sudden the characteristics of combining, under the conditions of varying environment, i.e., different generating regions, occurrence type is different, normal calamity Area is typically to break out occurrence type, even disaster area and without disaster area be generally progressive generation type, diffusion generation type and low-density stablize Generation type.On the one hand the reason of breaking out is that dendrolimus punctatus has as the hereditary capacity for breaking out kind, be on the other hand big face The presence of product Pinus massoniana forest.The startup factor broken out is high temperature and drought or the dynamic of the chaos as caused by environmental noise, is broken out Rising stage is that positive density dependent interaction drives, and declines phase and incubation period mainly by pine tree induction of resistance, serious mistake leaf and natural enemy The relevant effect of caused negative density.China shares 27 kinds of pine moth, but in this 27 kinds of pine moths only have 6 kinds often at Calamity, and the degree caused disaster of dendrolimus punctatus harm is classified as first, other kinds of sequence is dendrolimus sibiricus, dendrolimus tabulaeformis, red Pine moth, yunnan pine caterpillar, Dendrolimus kikuchii.Dendrolimus punctatus is liked eating old needle and not liking and eat the tender needle of children, due to old Needle moisture is few, and sour content is also lower, while cellulose, soluble-carbohydrate and protein content are higher, nutrients Matter is relatively abundant, facilitates the growth and development of pine moth.Masson pine extent of injury is higher, the egg laying amount of dendrolimus punctatus, pupal mass, Female ratio, breeding amount are lower, and the death rate is higher, and reason is mainly contained chemotrophy substance difference in needle.Currently, main logical It crosses to spray insecticide and be prevented and treated, although achieving many achievements, mainly be difficult to solve there is also Pesticide Residue, give it His species are with destructive destruction.In the local Yimeng Mountain Areas of the applicant, there is various masson pine forests, not only maintain The ecological balance, and it is also very popular to set the lower mushroom grown.Local horse hair pine tree is constantly by caterpillar in recent years Infringement, people are just prevented and treated using aerial spray, and caterpillar is under control quickly, even the orchard on periphery is without artificial application , the pest in orchard is also under control.Can with regard to recent years, applicants have discovered that, almost without mushroom under horse hair pine tree It grown, the cockroach, grasshopper on mountain largely reduce.After aerial spray, the applicant is into observing in mountain forest, not only hairiness Worm, cockroach, grasshopper die, and can also find the frog and bird to die.It is learnt after dissecting frog and bird, the cause of the death To have eaten caused by the toys such as the caterpillar poisoned with poison, cockroach, grasshopper.The large area of pesticide uses, serious to destroy life State balance, threatens the health of the mankind.Therefore, the applicant passes through the practice of many years, develops a kind of Control Dendrolimus punctatus Biological agent, by practice, which only has killing effect to dendrolimus punctatus, and pharmacological property is decomposed quickly, will not be to it He constitutes harm by animal.
Summary of the invention
The object of the present invention is to provide a kind of biological agents of Control Dendrolimus punctatus.
The purpose of the present invention is what is be achieved through the following technical solutions, the biological agent is by active constituent chlorine worm benzoyl Amine, biomass and auxiliary agent are made.
9-13 parts of the active constituent Rynaxypyr, 5-8 parts of biomass.
The auxiliary agent is by 2-3 parts of fatty alcohol polyoxyethylene ether, 0.4-1.2 parts of propylene glycol, 1.2-1.8 parts of pentaerythrite, poly- 1.5-2.5 parts of vinylpyrrolidone compositions.
The biomass is crushed after being mixed with chicken fiber crops by weight 1:2 by Rubus rufolanatus H. T. Chang, and 80% ethyl alcohol of 8 times of amounts is added, Heating and refluxing extraction 2 times, each 3h, filtering, decompression filtrate recycling ethanol obtains crude extract to no alcohol taste.Crude extract is taken to be configured to Liquid-to-solid ratio is the load solution that 1:5, pH are 5, passes through 732 type cation exchange resins, using 4% ammonium hydroxide as eluant, eluent, 5BV/h Flow velocity eluted, eluent recycling design is to get biomass of the present invention.
The preparation of biological agent of the present invention: by weighed Rynaxypyr, fatty alcohol polyoxyethylene ether and pentaerythrite It is added in reaction kettle, being heated to 60 DEG C with the speed of 20 DEG C/min melts raw medicine, and stirs evenly and oily phase is made.It will be weighed Propylene glycol, polyvinylpyrrolidone, biomass and water are uniformly mixed, and are heated slowly to 70 DEG C, and water phase is made.Oil is mutually slow It injects in water phase, is sheared using high-speed intermittent cutter, shear time is 60-80 minutes, and cools down to room temperature, is made Obtain biological agent of the present invention.
Specific embodiment
Embodiment one: the biological pesticide is by Rynaxypyr raw medicine 13g, fatty alcohol polyoxyethylene ether 3g, propylene glycol 1.2g, pentaerythrite 1.8g, polyvinylpyrrolidone 2.5g, biomass 8g are made.The biomass is by Rubus rufolanatus H. T. Chang and chicken fiber crops By weight crushing after 1:2 mixing, 80% ethyl alcohol of 8 times of amounts is added, heating and refluxing extraction 2 times, each 3h, filtering, filtrate subtracts It pushes back and receives ethyl alcohol to no alcohol taste, obtain crude extract.Taking crude extract to be configured to liquid-to-solid ratio is the load solution that 1:5, pH are 5, passes through 732 Type cation exchange resin, using 4% ammonium hydroxide as eluant, eluent, the flow velocity of 5BV/h is eluted, eluent recycling design to get Biomass of the present invention.Weighed Rynaxypyr, fatty alcohol polyoxyethylene ether and pentaerythrite are added in reaction kettle, with 20 DEG C/speed of min is heated to 60 DEG C melts raw medicine, and stir evenly and oily phase is made.By weighed propylene glycol, polyvinyl pyrrole Alkanone, biomass and water are uniformly mixed, and are heated slowly to 70 DEG C, and water phase is made.Oil is mutually slowly injected into water phase, height is used The intermittent cutter of speed is sheared, and shear time is 70 minutes, and cools down to room temperature, and biological agent of the present invention is made.
Embodiment two: the biological pesticide is by Rynaxypyr raw medicine 11g, fatty alcohol polyoxyethylene ether 2.5g, the third two Alcohol 0.8g, pentaerythrite 1.5g, polyvinylpyrrolidone 2g, biomass 6.5g are made, and preparation method is the same as embodiment one.
Embodiment three: the biological pesticide is by Rynaxypyr raw medicine 9g, fatty alcohol polyoxyethylene ether 2g, propylene glycol 0.4g, pentaerythrite 1.2g, polyvinylpyrrolidone 1.5g, biomass 5g are made, and preparation method is the same as embodiment one.
Heat storage stability test
With syringe by the clean ampoule bottle of 12g biological agent injection of the present invention, sealed rapidly with thermal-flame, after sealing Ampoule bottle be placed in 52 ± 4 DEG C of baking oven, it is static heat storage 15d after take out, detect appearance without layering, mobility, dispersibility, life The indices such as object activity are preceding unchanged with heat storage.Biological agent heat storage of the present invention is qualified.Its result is equivalent to storage at normal temperature 2 years Qualified products.
Low-temperature stability test
(sample contacts bottleneck will be avoided) in the clean ampoule bottle of 12g biological agent injection of the present invention with syringe, uses high temp fire Flame (alcohol blast burner) sealing (solvent is avoided to volatilize) rapidly, the ampoule bottle after sealing is placed under 0 DEG C of low temperature after cold storage 15d and is taken Out, for detection observation appearance without layering, the indices such as mobility, dispersibility, bioactivity are preceding unchanged with heat storage, are that low temperature is steady Qualitative qualification.
Freeze-thaw stability test
(sample contacts bottleneck will be avoided) in the clean ampoule bottle of 12g sample to be tested injection with syringe, with thermal-flame (alcohol Blowtorch) sealing (solvent is avoided to volatilize) rapidly, the ampoule bottle after sealing is placed under 20 DEG C of low temperature after 15h, ampoule bottle is taken out 8h at a temperature of being placed in 20 DEG C, this process are considered as one cycle, check after recycling in triplicate, and sample is precipitated without solid as qualification.
Dilution stability testing standard hard water: anhydrous calcium chloride 0.304g and the magnesium chloride 0.139g with the crystallization water are weighed In the volumetric flask of 1000mL, with distilled water dissolved dilution to graduation mark.
Measuring method: in 250mL beaker, being added 100mL28 DEG C of ± 3 DEG C of standard hard waters, is drawn in right amount originally with pipette Invention biological agent, is slowly added into hard water in the case where being stirred continuously, it is made to be made into 100mL emulsion.After adding, continue 20s is stirred with the speed of 4r/s, emulsion is moved into cleaning immediately, is dried in 100mL graduated cylinder, and graduated cylinder is placed in water bath with thermostatic control It is interior, within the scope of 30 DEG C ± 3 DEG C of temperature, 2h is stood, is taken out, observes emulsion in graduated cylinder without oil slick (cream), heavy oil and precipitating It is precipitated, then determines stability of emulsion for qualification.
Pourability test
Biological agent of the present invention is placed in the graduated cylinder (including plug) weighed, is attached at the 8/10 of graduated cylinder volume, stoppers mill Mouth plug, weighs, and places 30h.Plug is opened, graduated cylinder is tilted 45, topples over 2min, then be inverted 2min.Again weighing tank and plug Son.The water (20 DEG C) that will be equivalent to 80% graduated cylinder volume pours into graduated cylinder, grinding port plug is stoppered, after graduated cylinder is overturned 10 times, by upper It states operation and topples over content, third time weighs graduated cylinder and plug.Experimental result, the residue after toppling over is less than 5.0%, after washing Residue less than 0.5% for qualification.
Woodland pharmacodynamic test
Using by this bio-chemical control made of embodiment two be experimental group, using 3% high permeation fenoxycarb prevention and treatment be anti- It controls group, only use main ingredient Rynaxypyr raw medicine, be A according to the prevention and treatment of drug A made of the preparation method in embodiment Group only uses main ingredient biomass, is B group according to the prevention and treatment of drug B made of the preparation method in embodiment, each group dilutes 500 times of liquid.
Experimental field it is located at the masson pine forest encroached on by caterpillar Linyi City Yinan County, does not apply it before test and during test His pesticide.Temperature is at 26~33 degrees Celsius, 30 degrees Celsius of mean temperature during test;8 processing are set in this Field tests.Each Processing is repeated 2 times, totally 16 processing cells, is selected masson pine growing way and almost the same forest block medication of falling ill, is sprayed using backpack Day with fog, liquid volume standard are 2 liters/plant, and whole strain is uniform by medicine, and medical fluid is avoided to drift about.
Group Extension rate Method Preventive effect after for 24 hours Preventive effect after 72h
Experimental group 500 times of dilution Complete stool even spraying 91% 98%
Prevention and treatment group 500 times of dilution Complete stool even spraying 82% 88%
A group 500 times of dilution Complete stool even spraying 61% 65%
B group 500 times of dilution Complete stool even spraying 50% 54%
By being tested above it is found that the biological agent of the invention ability of killing caterpillar is most strong, ideal experiment is achieved Effect.
Indoor toxicity test: referring to FAO(FAO (Food and Agriculture Organization of the United Nation)) measuring method recommended, and improved.Three kinds of medicines The Toxicity Determination result such as following table of the agent to dendrolimus punctatus.
Medicament title Time/hour Virulence regression equation LC50 Co-toxicity coefficient
Biological agent 48 y=1.4021x+4.2113 3.68mg/L 140.1
Drug A 48 y=1.9568x+4.2323 31.11mg/L -
Drug B 48 y=1.6712x+3.6547 72.76mg/L -
It is mixed that biomass and Rynaxypyr in biological agent of the present invention are evaluated using the co-toxicity coefficient method of the abundant proposition of Sun Yun The synergy of agent, if the co-toxicity coefficient (CTC) of mixture less than 80, is antagonism;80~120 be summation action;It is greater than 120, it is synergistic effect.Therefore, main ingredient Rynaxypyr and the synergy of biomass mixture are in biological agent of the present invention Synergistic effect, this is consistent with the above experimental result.
Dead caterpillar feeding frog, pigeon, chicken are picked respectively, and observe the situation of change of frog, pigeon, chicken.
Medicine name Animal name Number of elements Caterpillar amount (/ gram) is fed daily 10th day 20th day
Biological agent group Frog 30 20 Without abnormal Without abnormal
Drug A group Frog 30 20 Dead 7 Dead 13
Drug B group Frog 30 20 Dead 2 Dead 4
Experiment is done to pigeon, chicken and achieves similar experiment as a result, it follows that biological agent of the invention, toxicity drop It is low, it is conducive to environmental protection and maintains the ecological balance.
In actual production, since mulberry tree bacterial blight has occurred in oneself mulberry trees garden of the applicant, I considers this hair The hypotoxicity of bright biological agent, with 700 times of liquid of biological agent of the invention, mulberry tree medication to bacterial blight occurs, liquid volume Standard is 45kg/ mus, and every plant of blade and stem are uniform by medicine.Second of medicine is applied after being spaced 7 days after being administered for the first time, is applied in every time It uniformly investigates within 7th day the state of an illness of mulberry tree bacterial blight after medicine afternoon, calculate disease index, control efficiency.
Mulberry tree bacterial blight incidence grade scale is as follows: severity Scaling standard: 0 grade, disease-free spot on branches and leaves;1 grade, scab Area accounts for entire 1/6 or less branches and leaves area;2 grades, lesion area accounts for the 1/6~1/4 of entire branches and leaves area;3 grades, lesion area accounts for The 1/4~1/2 of entire branches and leaves area;4 grades, lesion area accounts for 1/2 or more of entire branches and leaves area.
Disease refers to be calculated as follows with control efficiency:
Disease index (%)=Σ (the sick grade × disease grade number of blade) × 100/ highest disease grade × total leaf number.Control efficiency (%)= The control disease index of (control disease index-processing disease index) × 100/.
Experimental result: the mulberry tree control efficiency for reaching 2 grade standards to bacterial blight incidence is as follows.
By be administered situation above it is found that biological agent of the invention can effectively preventing mulberry tree bacterial blight, achieve reason Think control efficiency.During application, when feeding a small amount of silkworm of isolation using mulberry leaf, and it is no abnormal.

Claims (7)

1. a kind of biological agent of Control Dendrolimus punctatus, it is characterised in that the biological agent is by active constituent chlorine worm benzoyl Amine, biomass and auxiliary agent are made.
2. a kind of biological agent of Control Dendrolimus punctatus as described in claim 1, it is characterised in that the active constituent chlorine 9-13 parts of worm benzamide, 5-8 parts of biomass.
3. a kind of biological agent of Control Dendrolimus punctatus as described in claim 1, it is characterised in that the auxiliary agent is by fat 1.5-2.5 parts of 2-3 parts of alcohol polyoxyethylene ether, 0.4-1.2 parts of propylene glycol, 1.2-1.8 parts of pentaerythrite, polyvinylpyrrolidone groups At.
4. benefit require 1 described in a kind of biological agent of Control Dendrolimus punctatus, it is characterised in that the biomass is by red silk floss Rattan crushes after mixing with chicken fiber crops by weight 1:2, be added 8 times amount 80% ethyl alcohol, heating and refluxing extraction 2 times, each 3h, mistake Filter, decompression filtrate recycling ethanol obtain crude extract to no alcohol taste.
5. taking crude extract to be configured to liquid-to-solid ratio is the load solution that 1:5, pH are 5, by 732 type cation exchange resins, with 4% Ammonium hydroxide is eluted as eluant, eluent, the flow velocity of 5BV/h, and eluent recycling design is to get biomass of the present invention.
6. a kind of preparation method of the biological agent of Control Dendrolimus punctatus, it is characterised in that weighed Rynaxypyr, rouge Fat alcohol polyoxyethylene ether and pentaerythrite are added in reaction kettle, and being heated to 60 DEG C with the speed of 20 DEG C/min melts raw medicine, and It stirs evenly and oily phase is made;Weighed propylene glycol, polyvinylpyrrolidone, biomass and water are uniformly mixed, and are slowly heated To 70 DEG C, water phase is made.
7. oil is mutually slowly injected into water phase, to be sheared using high-speed intermittent cutter, shear time is 60-80 minutes, And room temperature is cooled down to, biological agent of the present invention is made.
CN201810890155.5A 2018-08-07 2018-08-07 A kind of biological agent and preparation method of Control Dendrolimus punctatus Pending CN109169733A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114402891A (en) * 2022-01-24 2022-04-29 重庆市林业科学研究院 Planting method for interplanting glede tea under degraded pinus massoniana forest

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Publication number Priority date Publication date Assignee Title
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Application publication date: 20190111