CN100450360C - Rotenone and dinotefuran mixed microemulsion and preparation method thereof - Google Patents
Rotenone and dinotefuran mixed microemulsion and preparation method thereof Download PDFInfo
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- CN100450360C CN100450360C CNB2006101235245A CN200610123524A CN100450360C CN 100450360 C CN100450360 C CN 100450360C CN B2006101235245 A CNB2006101235245 A CN B2006101235245A CN 200610123524 A CN200610123524 A CN 200610123524A CN 100450360 C CN100450360 C CN 100450360C
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Abstract
The invention discloses a rotenone and dinotefuran composite microemulsion and its preparing process, wherein the microemulsion comprises the constituents (by weight percent) of rotenone 0.5-25%, dinotefuran 1.5-45%, emulsifying agent 3-22%, penetrating agent 2-16%, stabilizing agent 1-15%, auxiliary solvent 2-20%, deionized water 22-72%. The preparation comprises the steps of stirring and mixing homogeneously, charging deionized water, stirring and mixing homogeneously again, then stewing for 5-12 hours, heating to 41-58 deg C, and sufficiently blending.
Description
Technical field
The present invention relates to the insecticide mixture technology, relate to rotenone and dinotefuran mixed pest killing micro emulsion and preparation method thereof particularly.
Background technology
In recent years, developed countries such as Great Britain and America are to an organic solvent restriction increasingly stringent in the pesticidal preparations, dimethylbenzene is disabled to be the solvent of agricultural chemicals, this is a kind of challenge to cream preparation, and wetting powder and pulvis can bring dust pollution, thereby impel agricultural chemicals to develop along efficient (super-high-efficient), low toxicity, safety, biorational and the good direction of Environmental compatibility.People are when strengthening the novel pesticide research and development, pay attention to research and development more to the formulations of pesticide, it wherein is the direction that the pesticides new formulation of base has become world's formulations of pesticide research and development with water, and as a kind of novel water-based pesticide formulation, a kind of so just environment friendly agricultural preparation of microemulsion.
Rotenone (rotenone) belongs to flavonoids, and its chemical name is 2R-(2 α, 6a α, 12a α)]-1,2.12,12a-tetrahydrochysene-8,9-dimethoxy-2-(1-methyl ethylene)-[I]-chromene [3,4-b]-furans is also-[2,3-h] [1]-chromene-6 (6aH)-ketone, be mainly derived from the plants such as trifoliate jewelvine, Africa mountain soya bean, its insecticidal action mechanism is special, insect is had strong stomach toxicity and contact toxicity, and have food refusal and the inhibition activity of growing concurrently.Can be used for the various pests control on vegetables, fruit tree, paddy rice, tea tree, tobacco and the cotton.But the rotenone product of using on the at present domestic and international agricultural chemicals market is many based on rotenone emulsifiable solution.
The chemical name of MTI-446 (dinotefuran) is (RS)-1-methyl-2-nitro-3-[(3-oxolane)-methyl] guanidine, it is to be developed the earliest by Mitsui chemical company, the third generation nicotinic insecticide of listing in 2002.Its insecticidal spectrum is wide, can prevent and treat various pests such as Semiptera, Lepidoptera and Hymenoptera, and has the significant interior osmosis of inhaling, and promptly shows insecticidal activity at very low dosage.This insecticide is fool proof to mammal, birds and aquatile, and crops are not had poisoning, can be used for the control of insect of numerous crops such as paddy rice, fruit tree and vegetables.But MTI-446 is the same with many chemical insecticides, and long-term, continuous, single use all can be developed immunity to drugs.And the formulation of the MTI-446 pesticide product of using on the present agricultural chemicals market mainly contains wetting powder, pulvis and granule.
Rotenone and dinotefuran mixed use can be worked in coordination with and played a role, and have remedied self deficiency of single agent agricultural chemicals.To at present, the bibliographical information of relevant rotenone of Shang Weijian and dinotefuran mixed microemulsion.
Summary of the invention
The objective of the invention is to overcome the rotenone product of using on the existing domestic and international agricultural chemicals market, based on rotenone emulsifiable solution, the formulation of MTI-446 pesticide product is mainly wetting powder, pulvis and granule, the shortcoming of the dust pollution that causes and the toxicity of cream preparation, provide a kind of high-efficiency low-toxicity, low cost, environmentally friendly supplying, the friendly pesticide species of enriched environment to cabbage aphid and significant rotenone of cucumber Bemisia tabaci control efficiency and dinotefuran mixed pest killing micro emulsion novel form agricultural chemicals.Another object of the present invention is to provide the preparation method of above-mentioned rotenone and dinotefuran mixed pest killing micro emulsion.
A kind of rotenone and dinotefuran mixed pest killing micro emulsion, by weight percentage, each component is in the prescription: rotenone 0.5-25%, MTI-446 1.5-45%, emulsifier 3-22%, bleeding agent 2-16%, stabiliser content 1-15%, cosolvent 2-20%, deionized water 22-72%.Used emulsifier can be selected from one or more in polyoxyethylene nonylphenol ether, phenethyl phenol polyethenoxy ether, xenol APEO and the benzylphenol APEO.Used bleeding agent is selected from one or more in sulfosuccinate di-sec-octyl sodium salt, octyl phosphate sodium salt and the azone.Used stabilizing agent is selected from one or more in butyl glycidyl ether, phenyl glycidyl ether and the acrylic glycidol ether.Used cosolvent can be selected from one or more in isoamyl alcohol, acetone, ethyl acetate and the phenol.
The preparation method of rotenone and dinotefuran mixed pest killing micro emulsion, step is as follows: earlier with rotenone and MTI-446, emulsifier, bleeding agent, stabilizing agent, cosolvent in high-speed shearing machine, after mixing, add deionized water again, mix, left standstill then 5-12 hour, be heated to 41-58 ℃, after fully stirring, can make rotenone and dinotefuran mixed pest killing micro emulsion.
The microemulsion that is mixed of the present invention is the microemulsion that contains active insecticidal components rotenone and MTI-446.The present invention utilizes derris root or Africa mountain soya bean blade to carry out lixiviate, and extract becomes the concentrated extract that contains rotenone behind concentrating under reduced pressure.
Compared with prior art, the present invention has following characteristics:
1. the present invention is a kind of new high-efficiency formulation of insecticides, and vegetable-crop pest-insects such as aphid and Bemisia tabaci are had significant drug effect.
2. formulation of insecticides of the present invention is difficult for producing poisoning to environment, people and animals and other beneficial organism safety.
3. each composition in the mixture can be worked in coordination with in application and be played a role, and has remedied self deficiency of single agent agricultural chemicals, uses such agricultural chemicals to be particularly suited for control and has produced serious drug-fast insect.
4. formulation of insecticides bin stability of the present invention is good, can deposit 1 year more than half.
5. formulation of insecticides of the present invention is with low cost, and preparing process is simple, is suitable for large scale application.
Embodiment
In order to understand the present invention better, the invention will be further described below in conjunction with embodiment, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Embodiment 1: take by weighing rotenone 0.5kg, MTI-446 45.0kg, after mixing in high-speed shearing machine with phenethyl phenol polyethenoxy ether 5.0kg, octyl phosphate sodium salt 3.0kg, butyl glycidyl ether 5.0kg, isoamyl alcohol 3.5kg then, add deionized water 38.0kg at last again, mix, left standstill 10 hours, be heated to 55 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 4800 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 87.3%, 83.5%, its 3400 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 90.2%, 85.3%.
Embodiment 2: take by weighing rotenone 0.6kg, MTI-446 44.0kg, after mixing in high-speed shearing machine with phenethyl phenol polyethenoxy ether 2.0kg, polyoxyethylene nonylphenol ether 2.5kg, benzylphenol APEO 1.5kg, octyl phosphate sodium salt 2.0kg, butyl glycidyl ether 5.0kg, isoamyl alcohol 4.5kg then, add deionized water 37.9kg at last again, mix, left standstill 11 hours, be heated to 53 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 4800 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 90.5%, 88.0%, its 3400 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 91.3%, 87.5%.
Embodiment 3: take by weighing rotenone 25.0kg, MTI-446 1.5kg, after mixing in high-speed shearing machine with phenethyl phenol polyethenoxy ether 6.0kg, polyoxyethylene nonylphenol ether 6.5kg, sulfosuccinate di-sec-octyl sodium salt 7.0kg, azone 8.0kg, butyl glycidyl ether 5.0kg, phenyl glycidyl ether 6.0kg, acetone 6.0kg then, add deionized water 29.0kg at last again, mix, left standstill 7 hours, be heated to 56 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 3500 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 93.2%, 88.7%, its 2500 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 90.7%, 84.4%.
Embodiment 4: take by weighing rotenone 23.2kg, MTI-446 2.2kg, after mixing in high-speed shearing machine with benzylphenol APEO 7.0kg, polyoxyethylene nonylphenol ether 4.5kg, octyl phosphate sodium salt 13.0kg, butyl glycidyl ether 5.0kg, acrylic glycidol ether 7.0kg, ethyl acetate 4.5kg then, add deionized water 33.6kg at last again, mix, left standstill 8 hours, be heated to 57 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 3500 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 94.6%, 90.8%, its 2500 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 94.1%, 91.9%.
Embodiment 5: take by weighing rotenone 13.2kg, MTI-446 22.5kg, after mixing in high-speed shearing machine with benzylphenol APEO 5.0kg, octyl phosphate sodium salt 10.5kg, phenyl glycidyl ether 4.0kg, ethyl acetate 4.5kg, isoamyl alcohol 1.5kg then, add deionized water 38.8kg at last again, mix, left standstill 12 hours, be heated to 58 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 3500 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 94.5%, 90.3%, its 2500 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 93.4%, 87.7%.
Embodiment 6: take by weighing rotenone 7.5kg, MTI-446 10.0kg, then with polyoxyethylene nonylphenol ether 2.0kg, phenethyl phenol polyethenoxy ether 1.0kg, xenol APEO 1.5kg, sulfosuccinate di-sec-octyl sodium salt 7.0kg, butyl glycidyl ether 2.5kg, phenyl glycidyl ether 2.5kg, acrylic glycidol ether 4.0kg, acetone 4.0kg, after phenol 2.0kg mixes in high-speed shearing machine, add deionized water 56.0kg at last again, mix, left standstill 11 hours, be heated to 51 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 2500 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 94.2%, 88.7%, its 1400 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 93.4%, 90.2%.
Embodiment 7: take by weighing rotenone 5.2kg, MTI-446 20.5kg, after mixing in high-speed shearing machine with xenol APEO 17.5kg, sulfosuccinate di-sec-octyl sodium salt 3.2kg, azone 3.0kg, butyl glycidyl ether 4.0kg, acrylic glycidol ether 3.0kg, acetone 2.5kg, ethyl acetate 6.0kg then, add deionized water 35.1kg at last again, mix, left standstill 7 hours, be heated to 46 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 3000 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 95.5%, 93.2%, its 2000 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 91.2%, 87.5%.
Embodiment 8: take by weighing rotenone 20.0kg, MTI-446 4.8kg, after mixing in high-speed shearing machine with benzylphenol APEO 6.0kg, octyl phosphate sodium salt 5.0kg, butyl glycidyl ether 2.0kg, acrylic glycidol ether 4.5kg, phenol 15.0kg then, add deionized water 42.7kg at last again, mix, left standstill 10 hours, be heated to 45 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 3000 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 93.3%, 86.7%, its 2200 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 89.4%, 86.5%.
Embodiment 9: take by weighing rotenone 15.8kg, MTI-446 2.7kg, after mixing in high-speed shearing machine with benzylphenol APEO 9.0kg, octyl phosphate sodium salt 3.8kg, azone 4.5kg, phenyl glycidyl ether 5.0kg, acetone 8.5kg then, add deionized water 50.7kg at last again, mix, left standstill 7 hours, be heated to 58 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 3000 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 90.7%, 84.4%, its 2200 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 83.2%, 81.7%.
Embodiment 10: take by weighing rotenone 11.0kg, MTI-446 2.0kg, after mixing in high-speed shearing machine with xenol APEO 4.2kg, benzylphenol APEO 6.8kg, octyl phosphate sodium salt 5.5kg, azone 3.5kg, acrylic glycidol ether 6.0kg, ethyl acetate 12.0kg, add deionized water 49.0kg at last again, mix, left standstill 8 hours, be heated to 57 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 2000 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 92.8%, 88.4%, its 1200 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 87.3%, 82.6%.
Embodiment 11: take by weighing rotenone 6.5kg, MTI-446 6.7kg, after mixing in high-speed shearing machine with xenol APEO 4.0kg, benzylphenol APEO 6.0kg, octyl phosphate sodium salt 3.8kg, sulfosuccinate di-sec-octyl sodium salt 3.5kg, azone 3.2kg, phenyl glycidyl ether 4.0kg, ethyl acetate 5.0kg then, add deionized water 57.3kg at last again, mix, left standstill 9 hours, be heated to 41 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 2500 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 94.6%, 93.7%, its 1200 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 96.1%, 88.5%.
Embodiment 12: take by weighing rotenone 1.5kg, MTI-446 30.0kg, after mixing in high-speed shearing machine with xenol APEO 8.0kg, benzylphenol APEO 9.0kg, octyl phosphate sodium salt 3.2kg, azone 5.0kg, phenyl glycidyl ether 4.0kg, ethyl acetate 4.2kg, isoamyl alcohol 3.0kg, phenol 2.6kg then, add deionized water 29.5kg at last again, mix, left standstill 10 hours, be heated to 43 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 3200 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 96.2%, 93.5%, its 2400 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 93.2%, 88.7%.
Embodiment 13: take by weighing rotenone 2.7kg, MTI-446 14.2kg, after mixing in high-speed shearing machine with benzylphenol APEO 3.5kg, azone 10.0kg, butyl glycidyl ether 9.0kg, isoamyl alcohol 7.0kg then, add deionized water 53.6kg at last again, mix, left standstill 7 hours, be heated to 42 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 2500 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 91.6%, 87.5%, its 1400 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 95.7%, 90.3%.
Embodiment 14: take by weighing rotenone 5.5kg, MTI-446 41.0kg, after mixing in high-speed shearing machine with phenethyl phenol polyethenoxy ether 3.0kg, benzylphenol APEO 7.4kg, sulfosuccinate di-sec-octyl sodium salt 3.5kg, octyl phosphate sodium salt 3.5kg, azone 2.0kg, phenyl glycidyl ether 3.5kg, butyl glycidyl ether 1.2kg, phenol 6.0kg then, add deionized water 23.4kg at last again, mix, left standstill 10 hours, be heated to 50 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 4500 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 98.5%, 93.2%, its 3500 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 96.7%, 94.8%.
Embodiment 15: take by weighing rotenone 15.0kg, MTI-446 32.0kg, after mixing in high-speed shearing machine with phenethyl phenol polyethenoxy ether 7.0kg, sulfosuccinate di-sec-octyl sodium salt 2.5kg, octyl phosphate sodium salt 4.5kg, azone 2.5kg, acrylic glycidol ether 5.0kg, acetone 3.5kg, phenol 4.5kg then, add deionized water 23.5kg at last again, mix, left standstill 11 hours, be heated to 52 ℃, after fully stirring, promptly can be made into microemulsion.The dilute with water said preparation carries out field control effectiveness test, its 3500 times of liquid to the cabbage aphid medicine after the control efficiency of the 7th day and 14 days be respectively 97.5%, 91.3%, its 2400 times of liquid to cucumber Bemisia tabaci medicine after the control efficiency of the 7th day and 14 days be respectively 94.6%, 93.0%.
The foregoing description shows, rotenone of the present invention and the dinotefuran mixed microemulsion not only control efficiency to cabbage aphid and cucumber Bemisia tabaci are remarkable, and this microemulsion is base with water, overcome the shortcoming that wetting powder and pulvis bring dust pollution, to environment, people and animals and other beneficial organism safety, be difficult for producing poisoning, and insect is difficult for it is developed immunity to drugs.Each composition in the mixture can be worked in coordination with in application and be played a role, and has remedied self deficiency of single agent agricultural chemicals, and has reduced the field pesticides amount of application, has reduced production cost of products.In addition, microemulsion bin stability of the present invention is good, can deposit 1 year more than half, and its preparation technology is simple, is suitable for large scale application.
Claims (2)
1, a kind of rotenone and dinotefuran mixed pest killing micro emulsion, it is characterized in that by weight percentage, each component is in the prescription: rotenone 0.5-25%, MTI-446 1.5-45%, emulsifier 3-22%, bleeding agent 2-16%, stabiliser content 1-15%, cosolvent 2-20%, deionized water 22-72%; Described emulsifier is selected from one or more in polyoxyethylene nonylphenol ether, phenethyl phenol polyethenoxy ether, xenol APEO and the benzylphenol APEO; Described bleeding agent is selected from one or more in sulfosuccinate di-sec-octyl sodium salt, octyl phosphate sodium salt and the azone; Described stabilizing agent is selected from one or more in butyl glycidyl ether, phenyl glycidyl ether and the acrylic glycidol ether; Described cosolvent is selected from one or more in isoamyl alcohol, acetone, ethyl acetate and the phenol.
2, the preparation method of described rotenone of claim 1 and dinotefuran mixed pest killing micro emulsion, it is characterized in that step is as follows: earlier with rotenone and MTI-446, emulsifier, bleeding agent, stabilizing agent, cosolvent in high-speed shearing machine, after mixing, add deionized water again, mix, left standstill then 5-12 hour, be heated to 41-58 ℃, after fully stirring, can make rotenone and dinotefuran mixed pest killing micro emulsion.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101700034B (en) * | 2009-08-01 | 2013-02-13 | 深圳诺普信农化股份有限公司 | Pesticide composition |
| CN101971831A (en) * | 2010-10-20 | 2011-02-16 | 华南理工大学 | Flubendiamide and rotenone combined insecticidal microemulsion and preparation method thereof |
| CN101971832A (en) * | 2010-10-20 | 2011-02-16 | 华南理工大学 | Compounded pesticidal microemulsion of chlorantraniliprole and rotenone and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH05255006A (en) * | 1991-12-20 | 1993-10-05 | American Cyanamid Co | Method and composition containing insecticide and stilbene compound for enhanced insecticidal activity |
| CN1309910A (en) * | 2001-02-20 | 2001-08-29 | 华南农业大学 | Mixed rotenone preparation |
| WO2005118552A2 (en) * | 2004-04-13 | 2005-12-15 | E.I. Dupont De Nemours And Company | Anthranilamide insecticides |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05255006A (en) * | 1991-12-20 | 1993-10-05 | American Cyanamid Co | Method and composition containing insecticide and stilbene compound for enhanced insecticidal activity |
| CN1309910A (en) * | 2001-02-20 | 2001-08-29 | 华南农业大学 | Mixed rotenone preparation |
| WO2005118552A2 (en) * | 2004-04-13 | 2005-12-15 | E.I. Dupont De Nemours And Company | Anthranilamide insecticides |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102415405B (en) * | 2011-10-31 | 2014-06-11 | 联保作物科技有限公司 | Dinotefuran micron-emulsion and preparation method thereof |
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