CN114847282B - Microcapsule suspending agent containing spinosad and preparation method thereof - Google Patents
Microcapsule suspending agent containing spinosad and preparation method thereof Download PDFInfo
- Publication number
- CN114847282B CN114847282B CN202210477817.2A CN202210477817A CN114847282B CN 114847282 B CN114847282 B CN 114847282B CN 202210477817 A CN202210477817 A CN 202210477817A CN 114847282 B CN114847282 B CN 114847282B
- Authority
- CN
- China
- Prior art keywords
- spinosad
- microcapsule
- agent
- suspending agent
- initiator
- Prior art date
- 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.)
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- JFLRKDZMHNBDQS-UCQUSYKYSA-N CC[C@H]1CCC[C@@H]([C@H](C(=O)C2=C[C@H]3[C@@H]4C[C@@H](C[C@H]4C(=C[C@H]3[C@@H]2CC(=O)O1)C)O[C@H]5[C@@H]([C@@H]([C@H]([C@@H](O5)C)OC)OC)OC)C)O[C@H]6CC[C@@H]([C@H](O6)C)N(C)C.CC[C@H]1CCC[C@@H]([C@H](C(=O)C2=C[C@H]3[C@@H]4C[C@@H](C[C@H]4C=C[C@H]3C2CC(=O)O1)O[C@H]5[C@@H]([C@@H]([C@H]([C@@H](O5)C)OC)OC)OC)C)O[C@H]6CC[C@@H]([C@H](O6)C)N(C)C Chemical compound CC[C@H]1CCC[C@@H]([C@H](C(=O)C2=C[C@H]3[C@@H]4C[C@@H](C[C@H]4C(=C[C@H]3[C@@H]2CC(=O)O1)C)O[C@H]5[C@@H]([C@@H]([C@H]([C@@H](O5)C)OC)OC)OC)C)O[C@H]6CC[C@@H]([C@H](O6)C)N(C)C.CC[C@H]1CCC[C@@H]([C@H](C(=O)C2=C[C@H]3[C@@H]4C[C@@H](C[C@H]4C=C[C@H]3C2CC(=O)O1)O[C@H]5[C@@H]([C@@H]([C@H]([C@@H](O5)C)OC)OC)OC)C)O[C@H]6CC[C@@H]([C@H](O6)C)N(C)C JFLRKDZMHNBDQS-UCQUSYKYSA-N 0.000 title claims abstract description 80
- 239000005930 Spinosad Substances 0.000 title claims abstract description 80
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- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 15
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- 239000002518 antifoaming agent Substances 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 10
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 9
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- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 7
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 6
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
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- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- OIPILFWXSMYKGL-UHFFFAOYSA-N acetylcholine Chemical compound CC(=O)OCC[N+](C)(C)C OIPILFWXSMYKGL-UHFFFAOYSA-N 0.000 description 2
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- 229960002715 nicotine Drugs 0.000 description 2
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 2
- 239000012053 oil suspension Substances 0.000 description 2
- 230000002688 persistence Effects 0.000 description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
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- 238000013112 stability test Methods 0.000 description 2
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- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 238000010257 thawing Methods 0.000 description 2
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- ZXQYGBMAQZUVMI-RDDWSQKMSA-N (1S)-cis-(alphaR)-cyhalothrin Chemical compound CC1(C)[C@H](\C=C(/Cl)C(F)(F)F)[C@@H]1C(=O)O[C@@H](C#N)C1=CC=CC(OC=2C=CC=CC=2)=C1 ZXQYGBMAQZUVMI-RDDWSQKMSA-N 0.000 description 1
- QFBCQOXKGBYUSU-UHFFFAOYSA-M 2-acetyloxyethyl(trimethyl)azanium;pyridine-3-carboxylate Chemical compound [O-]C(=O)C1=CC=CN=C1.CC(=O)OCC[N+](C)(C)C QFBCQOXKGBYUSU-UHFFFAOYSA-M 0.000 description 1
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- 241001414720 Cicadellidae Species 0.000 description 1
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 1
- 241000255925 Diptera Species 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
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- 239000005906 Imidacloprid Substances 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
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- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 description 1
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- 238000010521 absorption reaction Methods 0.000 description 1
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- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- RRZXIRBKKLTSOM-XPNPUAGNSA-N avermectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 RRZXIRBKKLTSOM-XPNPUAGNSA-N 0.000 description 1
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- 230000010534 mechanism of action Effects 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
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- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 1
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Classifications
-
- 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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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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
- 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
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/22—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom rings with more than six members
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
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Abstract
The invention discloses a microcapsule suspending agent containing spinosad and a preparation method thereof. The invention relates to a spinosad microcapsule suspending agent, which comprises a microcapsule, an auxiliary agent and water, wherein the microcapsule comprises a microcapsule wall and a microcapsule core, and the microcapsule core consists of spinosad raw medicine and a solvent; the capsule wall is a high molecular polymer obtained by polymerizing monomers under the action of an initiator. The spinosad microcapsule suspending agent disclosed by the invention can be stably dispersed and suspended in water, and the appearance is milky white homogeneous suspension liquid. The spinosad microcapsule suspending agent has good control effects on caterpillars, leaf miners, thrips, leaf eating beetles and the like, can delay the generation of drug resistance, reduce the pollution to the environment and has longer lasting period.
Description
Technical Field
The present disclosure relates to the field of pesticide formulation processing technology, and in particular, to a microcapsule suspension containing spinosad and a preparation method thereof.
Background
Spinosad is a macrolide nuisance-free high-efficiency biological pesticide extracted from Spinosad fermentation liquor. The spinosyn-producing parent strain, actinomycetes spinosad, was originally isolated from a waste brewery site in the Caribbean. Spinosad has a novel mode of action and can continuously activate target insect acetylcholine nicotinic receptors, but its binding site is different from that of nicotine and roar. Spinosad can also affect GABA receptors, but the mechanism of action is unclear. It is currently unknown whether there is cross-resistance to other types of pesticides. These compounds can cause rapid death of target phytophagous insects such as caterpillars, leaf miner, thrips leaf eating beetles, although regulatory authorities strongly require that the moderate residual activity of the compounds reduce the likelihood of resistance and swarming when resistance is not present. An effector of nicotinic acid acetylcholine receptors can continuously activate target insect acetylcholine nicotinic receptors, but its binding site is different from that of nicotine and imidacloprid. Spinosad can also influence GABA receptors, has rapid contact and stomach toxicity effects on pests, has strong penetration effect on leaves, can kill pests below epidermis, has longer residual period, and has a certain ovicidal effect on some pests. No internal absorption. Can effectively prevent and treat lepidoptera, diptera and seiulus pests, can well prevent and treat certain large amount of leaf feeding pest species in lepidoptera and orthoptera, and has poor prevention and treatment effects on piercing-sucking pests and mites. The pesticide composition is safe to predatory natural enemy insects, and has a unique insecticidal action mechanism, so that reports of cross resistance with other pesticides are not found at present. Is safe and harmless to plants. Is suitable for vegetables, fruit trees, gardening and crops. Can rapidly paralyze and paralyze phlegm of pests, and finally cause death. The insecticidal speed is comparable to chemical pesticides. The pesticide has high safety, has no cross resistance with the existing common pesticides, is a low-toxicity, high-efficiency and low-residue biological pesticide, has high-efficiency insecticidal performance and safety to beneficial insects and mammals, and is most suitable for producing pollution-free vegetables and fruits. However, the conventional general method for preparing the spinosad microcapsule suspending agent often has the problems of poor encapsulation effect, poor stability and short duration of action, for example, the duration of action of the microcapsule suspending agent of spinosad prepared by the general method is often only 7 days.
Disclosure of Invention
In order to solve the problems, the invention aims to provide the spinosad microcapsule suspending agent with high encapsulation efficiency, good stability and long lasting period and the preparation method thereof.
The invention provides a spinosad microcapsule suspending agent, which comprises a microcapsule, an auxiliary agent and water, wherein the microcapsule comprises a microcapsule wall and a microcapsule core, and the microcapsule core consists of spinosad raw medicine and a solvent; the capsule wall is a high molecular polymer obtained by polymerizing monomers under the action of an initiator.
Preferably, the monomer is selected from one or more of styrene, butadiene, ethylene, methacrylate, vinyl chloride, vinyl acetate, acrylonitrile, methacrylic acid;
preferably, the initiator is selected from one or more of azobisisobutyronitrile, azobisisoheptonitrile, azobisisovaleronitrile, sodium persulfate, potassium persulfate;
more preferably, the mass fraction ratio of monomer to initiator is from 1 to 10:1.
more preferably, the present invention provides a spinosad microcapsule suspension as follows:
spinosad 1-10%
Monomers 0.5-2.0%
Initiator 0.3-0.5%
1-30% of organic solvent
1-10% of surfactant
0.1-2% of thickener
3-10% of antifreezing agent
The water balance (complement 100%)
The invention also provides a preparation method of the spinosad microcapsule suspending agent, which comprises the following steps:
(1) Mixing spinosad, a solvent and a monomer to obtain a first material;
(2) Mixing water, a defoaming agent and an emulsifying agent to obtain a second material;
(3) Pouring the first material into the second material, and shearing to obtain a third material;
(4) Dropwise adding an initiator into the third material, mixing, heating and preserving heat to obtain a fourth material;
(5) And adding a thickening agent, an antifreezing agent and a dispersing agent into the fourth material to obtain the spinosad microcapsule suspending agent.
On the other hand, the invention also provides an application of the spinosad microcapsule suspending agent in controlling pests in agriculture and forestry.
Advantageous effects
1. The spinosad microcapsule suspending agent has good encapsulation effect, good stability and long lasting time;
2. the spinosad microcapsule suspending agent is more suitable for the comprehensive control of various pests in agriculture and forestry
3. The spinosad microcapsule suspending agent disclosed by the invention is simple in preparation process, energy-saving and environment-friendly.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. Throughout the specification and claims, unless explicitly stated otherwise, the term "comprise" or variations thereof such as "comprises" or "comprising" and the like will be understood to include the stated element without excluding the presence of other material elements.
In addition, numerous specific details are set forth in the following description in order to provide a better illustration of the invention.
It will be understood by those skilled in the art that the present invention may be practiced without some of these specific details. In some embodiments, materials, methods, means, etc. well known to those skilled in the art are not described in detail in order to highlight the gist of the present invention.
The invention provides a spinosad microcapsule suspending agent, which comprises a microcapsule, an auxiliary agent and water, wherein the microcapsule comprises a microcapsule wall and a microcapsule core, and the microcapsule core consists of spinosad raw medicine and a solvent; the capsule wall is a high molecular polymer obtained by polymerizing monomers under the action of an initiator.
The researchers of the present invention find that the general method for preparing the microcapsule suspending agent by using spinosad has defects in the aspects of encapsulation efficiency, stability and persistence, such as, but not limited to, poor encapsulation effect, poor stability and poor persistence. Researchers have unexpectedly found that the use of certain monomers to polymerize directly with an initiator can solve the above problems.
The monomer is one or more selected from styrene, ethylene, butadiene, methacrylate, vinyl chloride, vinyl acetate, acrylonitrile and methacrylic acid. The research shows that the selection of the monomer has a certain correlation on the effect of the product, and the experimental result shows that the ethylene, the butadiene and the methacrylic acid can obtain excellent effects. Therefore, the monomer of the present invention is preferably one of ethylene, butadiene, and methacrylic acid.
The initiator comprises one or more of azodiisobutyronitrile, azodiisoheptonitrile, azodiisovaleronitrile, sodium persulfate and potassium persulfate; the selection of the initiator directly influences the formation effect of the capsule wall and also influences the encapsulation effect of the microcapsule, and researches show that for the spinosad microcapsule suspension, sodium persulfate, azodiisovaleronitrile and azodiisobutyronitrile can be used as the initiator to obtain a better microcapsule suspension product.
Researchers in this invention have also found that the ratio of monomer to initiator affects the properties of the final product. The researchers have surprisingly found that the ratio of the total mass of polymer monomer and initiator is 1-10:1, a step of; optionally 5-10:1, a step of; further alternatively 6:1. within the above range, a product of the spinosad microcapsule suspension having excellent quality will be obtained.
The drug loading of the microcapsule suspending agent product is often an index for evaluating the quality of the product, and the higher the drug loading is, the better the effect of the product is. However, the inventors have surprisingly found that the higher the drug loading of spinosad prepared by the process of the present invention is, the better the drug loading is, and the lower the drug loading is, the better the drug loading is. The best results are only achieved if spinosad is in a certain range. The mass of the spinosad in the spinosad microcapsule suspending agent is 1-10% of the total mass fraction, preferably 5-10%; most preferably 8%, and the results of the study show that the above range has a good effect, and when the range is exceeded, the performance of the product will deteriorate.
The solvent in the spinosad microcapsule suspending agent comprises one or more of toluene, xylene, solvent oil, soybean oil, cyclohexanone, dimethyl sulfoxide, ethyl acetate, sec-butyl acetate and carbon tetrachloride; optionally xylene.
Further, the ratio of the total mass of spinosad and solvent in the spinosad microcapsule suspension is 1:1-10; preferably 1:1-5; more preferably 1:3.75.
further, the auxiliary agent in the above scheme includes an antifoaming agent, an emulsifying agent, a thickening agent, an antifreezing agent and a dispersing agent.
The defoaming agent is one or more selected from polyether defoaming agents and organic silicon defoaming agents;
the dispersing agent is one or more of sulfuric acid ester dispersing agent, polyether dispersing agent, benzyl naphthalene sulfonic acid formaldehyde condensate, lignin sulfonate, polycarboxylate, EO-PO segmented copolymer and phosphoric acid ester dispersing agent;
the thickener is one or more selected from aluminum magnesium silicate, xanthan gum, bentonite and white carbon black;
the antifreezing agent is one or more selected from ethylene glycol, propylene glycol and glycerol;
the emulsifier is one or more selected from fatty alcohol polyoxyethylene ether, block polyether, alkylphenol polyoxyethylene ether, sorbitan monostearate polyoxyethylene ether, castor oil polyoxyethylene ether, sodium lauryl sulfate, pesticide emulsion 500#, 601, BY110, NP-10 and Tween 60.
In the further scheme, the mass ratio of water, the defoamer, the emulsifier, the thickener, the dispersant and the antifreezing agent is 1:0.001-0.05:0.05-0.2:0.001-0.05:0.01-0.1:0.01-0.15; alternatively 1:0.01-0.03:0.08-0.15:0.02-0.04:0.05-0.07:0.1-0.13.
The invention also provides a preparation method of the spinosad microcapsule suspending agent, which comprises the following steps:
(1) Mixing spinosad raw medicine, a solvent and a monomer to obtain a first material;
(2) Mixing water, a defoaming agent and an emulsifying agent to obtain a second material;
(3) Pouring the first material into the second material, and shearing to obtain a third material;
(4) Dropwise adding an initiator into the third material, mixing, heating and preserving heat to obtain a fourth material;
(5) And adding a thickening agent, an antifreezing agent and a dispersing agent into the fourth material to obtain the spinosad capsule suspending agent.
In the step (3), the shearing rate is 5000-20000r/min, and the shearing time is 1-10min; optionally, the shearing rate is 5000-15000r/min, and the shearing time is 2-5min; further alternatively, the shear rate is 10000r/min and the shear time is 5min.
In the step (4), an initiator is dripped into the third material under the stirring condition, and the stirring speed is 100-800r/min; optionally, the stirring speed is 200-500r/min; further alternatively, the stirring is at a rate of 300r/min. Heating at 30-60deg.C for 1-5 hr; optionally, the heating temperature is 30-50 ℃, and the heat preservation time is 2-3h; further alternatively, the heating temperature is 40℃and the incubation time is 2.5h.
The embodiment of the invention also provides application of the prepared spinosad microcapsule suspending agent in controlling pests in agriculture and forestry.
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. In the following examples, the raw materials were commercially available.
Wherein, the liquid crystal display device comprises a liquid crystal display device,
the CAS number of spinosad is 23184-66-9;
the CAS number for methacrylic acid is 79-41-4;
ethylene has a CAS number of 9010-79-1;
butadiene with CAS number 106-99-0
Sodium persulfate has CAS number 7775-27-1
Azodiisobutyronitrile has a CAS number of 78-67-1
The organic silicon defoamer is SAG-630 defoamer of the new material company of the Michaelsen, america;
block polyether is purchased from bamboo grease, and the model is 5050PB;
the polycarboxylate was purchased from He Ju, england, model Atlox 4913;
the fatty alcohol polyoxyethylene ether is purchased from Nanjing chemical industry Co., ltd, and the model is AEO-7;
alkylphenol ethoxylates are purchased from Nantong De Yi chemical industry Co., ltd, and the model is OP-10;
sorbitan monostearate polyoxyethylene ether was purchased from the company Heda, uk under the model Tween60;
castor oil polyoxyethylene ether was purchased from south-Beijing-ether-chemical-industry Co., ltd, and the model was BY110.
The present invention will be further illustrated by reference to examples, which are commercially available if the raw materials used in the examples are not specifically illustrated. Meanwhile, the embodiments are not to limit the scope of the present invention, but to describe the concept and gist of the present invention in more detail.
Example 1
A method for preparing a spinosad microcapsule suspension, the method comprising the steps of:
(1) Uniformly mixing 8g of spinosad raw material, 30g of dimethylbenzene and 1.8g of methacrylic acid until the raw material is completely dissolved, so as to obtain a first material;
(2) Uniformly mixing 50g of water, 0.7g of organosilicon defoamer and 3g of block polyether to obtain a second material;
(3) Starting a high-speed shearing machine, adding the first material obtained in the step (1) into the second material obtained in the step (2) at a rotating speed of 10000r/min, and shearing for 5min to obtain a third material;
(4) Stirring the third material at the stirring speed of 300r/min, adding 0.3g of sodium persulfate, and preserving the temperature at 40 ℃ for 2.5h to obtain a fourth material;
(5) Adding 0.2g of xanthan gum, 2g of polycarboxylate and 4g of ethylene glycol into the fourth material obtained in the step (4) to obtain a spinosad microcapsule suspending agent;
in the above examples, the mass ratio of the spinosad active compound to the solvent is 1:3.75;
the ratio of the total mass of polymer monomer and initiator was 6:1, a step of;
the ratio of spinosad to water total mass is 1:6.25;
the mass ratio of water, defoamer, emulsifier, thickener, dispersant and antifreezing agent is 1:0.014:0.06:0.004:0.04:0.8;
example 2
The difference with example 1 is that the dosage of spinosad is 1g, the dosage of No. 150 solvent oil is 37g, and the emulsifier is castor oil polyoxyethylene ether.
Example 3
The difference with example 1 is that the dosage of spinosad is 10g, the dosage of cyclohexanone is 20 g, and the emulsifier is fatty alcohol polyoxyethylene ether.
Example 4
The same as in example 1, except that the polymer monomer used was ethylene, the thickener was white carbon black, and the emulsifier was castor oil polyoxyethylene ether
Example 5
The difference from example 1 is that the polymer monomer used is butadiene, the antifreeze agent is ethylene glycol, and the thickener is magnesium aluminum silicate.
Example 6
The same as in example 1, except that the initiator used was azobisisobutyronitrile, the solvent was soybean oil, and the thickener was magnesium aluminum silicate
Example 7
The same as in example 1, except that the initiator used was azobisisovaleronitrile, the antifreeze agent was propylene glycol, and the emulsifier was castor oil polyoxyethylene ether
Comparative example 1
The same as in example 1, except that methacrylic acid was used in an amount of 3.6g
Comparative example 2
The same as in example 1, except that methacrylic acid was used in an amount of 0.6g
Comparative example 3
After screening each parameter, preparing the spinosad microcapsule suspending agent by using an interfacial polymerization method, wherein the method comprises the following steps of:
(1) Uniformly mixing 8g of spinosad raw material, 30g of dimethylbenzene and 1.5g of 2, 4-toluene diisocyanate until the spinosad raw material, and 10g of sorbitan monostearate polyoxyethylene ether to obtain a first material;
(2) 35.2g of water and 2g of organic silicon defoamer are mixed to obtain a second material;
(3) Starting a high-speed shearing machine, adding the first material obtained in the step (1) into the second material obtained in the step (2) at a rotating speed of 10000r/min, and shearing for 3min to obtain a third material;
(4) Stirring the third material at the stirring speed of 300r/min, dropwise adding 0.3g of diethylenetriamine, and preserving the temperature at 50 ℃ for 2.5h to obtain a fourth material;
(5) And (3) adding 3g of magnesium aluminum silicate, 5g of polycarboxylate and 5g of ethylene glycol into the fourth material in the step (4) to obtain the spinosad microcapsule suspending agent.
Comparative example 4
After screening the parameters, preparing the spinosad microcapsule suspending agent by using an in-situ polymerization method, wherein the method comprises the following steps of:
(1) Uniformly mixing 6g of melamine with 7.9g of formaldehyde solution with the concentration of 37 weight percent, and reacting for 1.5 hours at the pH value of 8 and the temperature of 70 ℃; 31.7g of water was added for dilution to obtain an aqueous solution of melamine-formaldehyde resin prepolymer.
(2) Uniformly mixing 8g of spinosad raw medicine and 30g of dimethylbenzene, and stirring to fully dissolve the spinosad raw medicine and the dimethylbenzene to obtain spinosad oil suspension;
(3) Uniformly mixing the melamine-formaldehyde resin prepolymer aqueous solution obtained in the step (1) and the spinosad oil suspension obtained in the step (2) to obtain a first material;
(4) Under the condition of room temperature, regulating the pH value to about 4.5, and uniformly adding acetic acid-sodium acetate buffer solution with the total concentration of 2 wt% into the first material obtained in the step (3) within 1h, uniformly mixing at the stirring speed of 1000r/min to regulate the pH value to 6.2, thereby obtaining a second material;
(5) Adding 5 wt% hydrochloric acid into the second material obtained in the step (4) at a constant speed within 1.5h at room temperature, and uniformly mixing at a stirring speed of 1200r/min to adjust the pH value to 3.3 to obtain a third material;
(6) Carrying out curing polycondensation on the third material obtained in the step (5) for 2 hours at the temperature of 60 ℃ to obtain a curing polycondensation product; and adjusting the pH of the cured polycondensation product to 7; 3g of magnesium aluminum silicate, 5.5g of polycarboxylate and 5g of ethylene glycol are added to obtain the spinosad microcapsule suspending agent.
Comparative example 5
After screening each parameter, preparing the spinosad suspending agent by a conventional method:
8g of spinosad raw material, 5g of sodium lignin sulfonate, 8g of block polyether, 1g of xanthan gum, 5g of ethylene glycol and 73g of water are uniformly mixed to obtain the spinosad suspending agent.
Comparative example 6
The difference is that the spinosad stock is used in an amount of 0.5g as in example 1.
Comparative example 7
The difference from example 1 is that the amount of spinosad stock is 11g.
Comparative example 8
The difference is that the initiator used is t-butyl hydroperoxide as in example 1.
Comparative example 9
The same as in example 1, except that the initiator used was ammonium persulfate.
Comparative example 10
The difference is that the monomer used is methylolacrylamide as in example 1.
Comparative example 11
The procedure is as in example 1, except that the monomer used is chloroprene.
Comparative example 12
The difference is that the active compound used is lambda-cyhalothrin as in example 1.
Comparative example 13
The difference is that the active compound used is avermectin as in example 1.
Test example 1
Measurement of microcapsule encapsulation Rate: the free spinosad content of the formulations of each of the examples and comparative examples was determined using high performance liquid chromatography and the encapsulation efficiency was calculated:
encapsulation efficiency (%) = (amount of active ingredient added-amount of free active ingredient)/amount of active ingredient added ×100%.
2, measuring heat storage stability: the formulations of each example and comparative example were placed in a container, sealed, placed in a constant temperature oven at (54.+ -. 2) °c, allowed to stand for 14 days, taken out, and observed for appearance.
3, freeze thawing stability measurement: the formulations of each example and comparative example were filled into containers; sealing, standing at-18deg.C for 18 hr, and standing at normal temperature for 8 hr; cycling for 4 times; after the cycle was completed, the appearance was observed.
The encapsulation efficiency and the storage stability test results are shown in Table 1. As shown in Table 1, compared with the comparative examples, the spinosad microcapsule suspending agent prepared by the method provided by the embodiment of the invention has high encapsulation efficiency and good heat storage and freeze thawing stability.
TABLE 1 encapsulation efficiency, storage stability test results
Test example 2
The test embodiment is experimentally arranged in a city of heng city of dune in Henan province, the crop to be tested is hot pepper, and the sowing mode is soil direct seeding; the test field has many perennial pests, and the main pests include cabbage caterpillar, cotton bollworm, leafhopper, plant bug, thrips and the like.
The experiment is carried out by setting 21 treatments, namely examples 1-7, comparative examples 1-13 and clear water comparison, repeating each treatment for 3 times, totally setting 63 cells, arranging random granules among the cells, planting capsicum in each cell in a dibbling mode, sowing 0.5kg capsicum seeds in each cell, and carrying out post-emergence pesticide application treatment. Plant treatment was performed using a hand-held compressed sprayer. The liquid medicine is prepared by adopting a two-step dilution method, and the water consumption is 40kg/667m 2 The method comprises the steps of carrying out a first treatment on the surface of the The dosage of the active ingredients per mu is 2g. And randomly taking 3 strains from each cell after 7d, 14d and 28d of the medicine, respectively investigating the number of live insects before and after the medicine, and calculating the death rate.
Mortality (%) = [ (number of live insects before drug-number of live insects after drug)/number of live insects before drug ] ×100%
Corrected mortality (%) = [ (treatment mortality-control mortality)/(100-control mortality) ]. 100%
Table 2 pharmacodynamic test of 7d, 14d, 28d after administration for controlling thrips Capsici fructus
| Treatment agent | 7d prevention effect after medicine (%) | 14d prevention effect after medicine (percent) | 28d prevention effect after medicine (%) |
| Example 1 | 99.5 | 99.7 | 99.4 |
| Example 2 | 98.6 | 97.1 | 95.3 |
| Example 3 | 97.9 | 95.8 | 93.7 |
| Example 4 | 99.1 | 94.6 | 90.8 |
| Example 5 | 98.2 | 94.9 | 91.0 |
| Example 6 | 97.3 | 95.6 | 92.9 |
| Example 7 | 98.0 | 94.9 | 91.8 |
| Comparative example 1 | 97.2 | 86.1 | 62.0 |
| Comparative example 2 | 94.7 | 82.9 | 68.4 |
| Comparative example 3 | 95.4 | 85.2 | 60.3 |
| Comparative example 4 | 96.3 | 80.5 | 68.3 |
| Comparative example 5 | 97.6 | 77.6 | 47.8 |
| Comparative example 6 | 90.2 | 50.5 | 30.8 |
| Comparative example 7 | 88.6 | 60.2 | 36.9 |
| Comparative example 8 | 87.7 | 71.3 | 55.4 |
| Comparative example 9 | 89.4 | 76.7 | 65.3 |
| Comparative example 10 | 90.1 | 79.9 | 63.7 |
| Comparative example 11 | 92.0 | 75.4 | 61.4 |
| Comparative example 12 | 92.6 | 78.8 | 70.5 |
| Comparative example 13 | 80.5 | 59.2 | 49.8 |
| Clear water control | - | - | - |
As can be seen from the table 2, the control effect time of the examples is longer, the death rate is higher, and the decrease starts 7 days after the other comparative examples are dosed, which shows that the duration of the spinosad microcapsule suspending agent prepared by the preparation method of the invention is longer.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (5)
1. The spinosad microcapsule suspending agent comprises a microcapsule, an auxiliary agent and water, wherein the microcapsule comprises a microcapsule wall and a microcapsule core, and is characterized in that the microcapsule core consists of spinosad raw medicine and a solvent; the capsule wall is a high molecular polymer obtained by polymerizing a monomer under the action of an initiator; the mass fraction of spinosad in the spinosad microcapsule suspending agent is 1% -10%; the mass fraction of the monomer in the spinosad microcapsule suspending agent is 1.8-2%, wherein the mass fraction ratio of the monomer to the initiator is 1-10:1, a step of; the monomer is selected from one of butadiene, ethylene and methacrylic acid; the initiator is selected from one or more of azodiisobutyronitrile, azodiisovaleronitrile and sodium persulfate; the solvent is selected from one or more of xylene, solvent oil, cyclohexanone and soybean oil.
2. The suspension of claim 1, wherein the adjuvant comprises an antifoaming agent, an emulsifying agent, a thickening agent, an antifreezing agent, and a dispersing agent; the defoaming agent is one or more selected from polyether defoaming agents and organic silicon defoaming agents; and/or the dispersing agent is one or more of sulfuric acid ester dispersing agent, polyether dispersing agent, benzyl naphthalene sulfonic acid formaldehyde condensate, lignin sulfonate, polycarboxylate, EO-PO block copolymer and phosphate dispersing agent; and/or the thickener is selected from one or more of magnesium aluminum silicate, xanthan gum, bentonite and white carbon black; and/or the antifreezing agent is selected from one or more of ethylene glycol, propylene glycol and glycerol; and/or the emulsifier comprises one or more of fatty alcohol polyoxyethylene ether, block polyether and castor oil polyoxyethylene ether.
3. A process for the preparation of a spinosad microcapsule suspension according to claim 1 or 2, characterized in that it comprises the following steps: (1) Mixing spinosad raw medicine, a solvent and a monomer to obtain a first material; (2) Mixing water, a defoaming agent and an emulsifying agent to obtain a second material; (3) Pouring the first material into the second material, and shearing to obtain a third material; (4) Dropwise adding an initiator into the third material, mixing, heating and preserving heat to obtain a fourth material; (5) And adding a thickening agent, an antifreezing agent and a dispersing agent into the fourth material to obtain the spinosad microcapsule suspending agent.
4. A process for the preparation of a spinosad microcapsule suspension according to claim 3, characterized in that: in the step (3), the shearing rate is 5000-20000r/min, and the shearing time is 1-10min; and/or, in the step (4), dropwise adding an initiator into the third material under stirring, wherein the stirring speed is 100-800r/min; the heating temperature is 30-60 ℃, and the heat preservation time is 1-4h.
5. Use of the spinosad microcapsule suspension of claim 1 or 2 for controlling pests in agriculture and forestry.
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Effective date of registration: 20240115 Address after: Building 5, No. 1500 Hangtang Road, Jinhui Town, Fengxian District, Shanghai, 2014 Patentee after: Yunfa Biotechnology (Shanghai) Co.,Ltd. Address before: 201400, No. 1500 Hangtang Road, Jinhui Town, Fengxian District, Shanghai Patentee before: Shanghai Mingdelida Biotechnology Co.,Ltd. |