CN110367250A - A kind of microcapsule formulations composition and preparation method thereof - Google Patents
A kind of microcapsule formulations composition and preparation method thereof Download PDFInfo
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- CN110367250A CN110367250A CN201910743469.7A CN201910743469A CN110367250A CN 110367250 A CN110367250 A CN 110367250A CN 201910743469 A CN201910743469 A CN 201910743469A CN 110367250 A CN110367250 A CN 110367250A
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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
- A01N25/26—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
-
- 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
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
-
- 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
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of microcapsule formulations compositions, include following components: the suspension for containing cyprodinil as inner aqueous phase, contain the suspension of epoxiconazole as outer aqueous phase, containing the oily phase of degradable high polymer material organic solvent, emulsifier, thickener, water.One aspect of the present invention will produce unexpected technical effect after the different two kinds of ingredients compounding of the mechanism of action, it was found that having significant synergies for wheat sharp eyespot, technical solution of the present invention improves drugloading rate by forming microcapsule formulations, it ensure that the validity of drug, while can be with Drug controlled release speed.
Description
Technical field
The present invention relates to a kind of compositions, more particularly to a kind of microcapsule formulations composition.
Background technique
Cyprodinil, the entitled Cyprodinil of English, chemical name are as follows: 4- cyclopropyl -6- Methyl-N-phenyl pyrimidine -2-
Amine is methionine biosynthesis inhibitor, is aminopyrimidine fungicide.Cyprodinil is a kind of broad spectrum activity contact sterilization agent, is had
Protection, treatment, blade penetrates and the activity of root interior suction, is mainly used for preventing and treating gray mold, scab, net blotch, glume blight
Etc. crop diseases.
Epoxiconazole, English name Cyproconazole, chemical name are as follows: 2- (4- chlorphenyl) -3- cyclopropyl -1- (1H-1,
2,4 triazol-1-yls) butyl- 2-2 alcohol, it is a kind of absorbability triazole bactericidal agent, mainly inhibits the synthesis of germ ergosterol,
The formation of germ cell wall is hindered, and epoxiconazole molecule has strength compatibility to fungal enzyme (14-dencthylase), with mesh
Preceding known fungicide is compared, and can effectively inhibit germ fungal pathogens, to banana, Kidney bean, melon, on peanut and other crops tikka
The diseases such as disease, powdery mildew, rust have good preventive effect.
Patent document CN105145583B discloses one kind containing Rynaxypyr microcapsule formulations and preparation method thereof, leads to
It crosses and Rynaxypyr is formed into microcapsule formulations, can be improved kernel drugloading rate, ensure that the validity of capsule.
Compound the document report for preventing and treating wheat sharp eyespot with epoxiconazole without open cyprodinil in the prior art,
The information of microcapsule formulations is formed after not having document report to compound the two.The present invention is by compounding shape with epoxiconazole for cyprodinil
At microcapsule formulations, on the one hand unexpected technical effect will be produced after the different two kinds of farm chemical ingredients compounding of the mechanism of action,
It was found that having significant synergies for wheat sharp eyespot, on the other hand, drugloading rate is improved by forming microcapsule formulations, is protected
The validity of drug is demonstrate,proved.
Summary of the invention
The purpose of the present invention is to provide a kind of microcapsule formulations composition pesticide containing cyprodinil and epoxiconazole includes
Have following components: the suspension for containing cyprodinil is as inner aqueous phase, the suspension for containing epoxiconazole as outer aqueous phase, containing can
The oily phase of degraded macromolecular material organic solvent, emulsifier, thickener, water.
In the inventive solutions, the quality hundred of the cyprodinil in the suspension of the inner aqueous phase cyprodinil
Score is 1-20%；
In the inventive solutions, the quality percentage of the epoxiconazole in the suspension of the outer aqueous phase epoxiconazole contains
Amount is 1%-20%；
In the inventive solutions, it is poly- to be selected from acylation chitosan, glycerine shell for the degradable high polymer material
Sugared, poly- (lactide-caprolactone) copolymer, polyglycolide, polylactic acid, appointing in poly- (own lactide-polyglycol ether) copolymer
It anticipates one kind or combinations thereof, wherein the mass percentage of the degradable high polymer material is 1-10%；
In the inventive solutions, the organic solvent appointing in dimethylbenzene, toluene, ethyl alcohol, cyclohexanone
It anticipates one kind or combinations thereof；
In the inventive solutions, the emulsifier is selected from amphiphilic polymer, preferably polyethyleneglycol first
One of ether-polylactic acid-glycollic acid, polyethylene glycol, Tween-80, polysorbate65 or any combination thereof object, the wherein matter of emulsifier
Amount percentage composition is 1-10%；
In the inventive solutions, the thickener is selected from carboxymethyl cellulose, Sodium Polyacrylate, polyacrylic acid
One of ester or any combination thereof, wherein the mass percentage of thickener is 1-10%；
It in the inventive solutions, further include stabilizer in the outer aqueous phase, wherein the stabilizer is selected from
One of polyvinyl alcohol, polyvinylpyrrolidone or combinations thereof, wherein the mass percentage of the stabilizer is 1-
10%.
In addition to this, the present invention also provides a kind of preparation methods of microcapsule formulations composition, it is characterised in that including such as
Lower step:
(1) cyprodinil is dispersed in water, cyprodinil suspension is obtained, as inner aqueous phase；
(2) epoxiconazole, stabilizer are dispersed in water, epoxiconazole suspension are obtained, as outer aqueous phase；
(3) degradable high polymer material is dissolved in organic solvent, obtains the organic solvent of degradable high polymer material
As oily phase；
(4) step (1) obtained inner aqueous phase and step (3) obtained oil are mixed, at the beginning of ultrasound obtains Water-In-Oil
Grade lotion；
(5) the obtained Water-In-Oil primary emulsion of step (4) is added in step (3) obtained outer aqueous phase, is passed through
Shaking table vibration is emulsified to obtain the water-oil-water type three-phase composite lotion；
(6) water-oil-water type three-phase composite lotion that step (5) obtains be stirred, be centrifuged, washed, be dried to obtain it is micro-
Capsule compositions.
In addition to this, the present invention also provides a kind of preparation methods of microcapsule formulations composition, it is characterised in that including such as
Lower step:
(1) cyprodinil is dispersed in water, cyprodinil suspension is obtained, as inner aqueous phase；The inner aqueous phase is phonetic
The mass percent of cyprodinil in the suspension of collarium amine is 1-20%；
(2) epoxiconazole, stabilizer are dispersed in water, epoxiconazole suspension are obtained, as outer aqueous phase；The outer aqueous phase
The mass percentage of epoxiconazole in the suspension of epoxiconazole is 1%-20%；
(3) degradable high polymer material is dissolved in organic solvent, obtains the organic solvent of degradable high polymer material
As oily phase；
(4) step (1) obtained inner aqueous phase and step (3) obtained oil are mixed, at the beginning of ultrasound obtains Water-In-Oil
Grade lotion；Wherein the oil is mutually and the volume ratio of inner aqueous phase is (1-20): (1-50), and the ultrasonic power is 100-
5000W, ultrasonic time are 10-30 seconds；Ultrasonic temperature is 25-50 DEG C；
(5) the obtained Water-In-Oil primary emulsion of step (4) is added in step (3) obtained outer aqueous phase, is passed through
Shaking table vibration is emulsified to obtain water-oil-water type three-phase composite lotion, the Water-In-Oil primary emulsion and foreign minister's water
Volume ratio be (1-10): (1-50), the time of vibration be 20-60min, temperature be 25-50 DEG C；
(6) water-oil-water type three-phase composite lotion that step (5) obtains is stirred, is centrifuged, washes and dries, obtains
The microcapsule formulations drug composition, wherein drying temperature is 40-60 DEG C.
In the inventive solutions, the mass percent of the cyprodinil in the suspension of inner aqueous phase cyprodinil is
1-20%, 2-15%, 5-10%, 5%, 8%, 10%, 15%, 20%；
In the inventive solutions, the mass percent of the cyprodinil in the suspension of outer aqueous phase epoxiconazole is 1-
20%, 2-15%, 5-10%, 5%, 8%, 10%, 15%, 20%；
In the inventive solutions, the degradable high polymer material in step (3) is selected from organic solvent dimethylbenzene, first
Any of or a combination of benzene, ethyl alcohol, cyclohexanone；And the mass-volume concentration of high molecular material is 1-200mg/mL, excellent
It is selected as 1-180mg/mL, 1-150mg/mL, 1-100mg/mL, 5-100mg/mL, 10-100mg/mL, 20-100mg/mL, 50-
100mg/mL；
In the inventive solutions, degradable high polymer material is selected from acylation chitosan, Glycerolchitosan, gathers
(lactide-caprolactone) copolymer, polyglycolide, polylactic acid, any one in poly- (own lactide-polyglycol ether) copolymer
Or combinations thereof, molecular weight 500-500000, preferably 1000-500000,5000-300000,10000-200000,
50000-100000；
In the inventive solutions, wherein step (2) it is obtained oil mutually and step (1) obtained inner aqueous phase
Volume ratio is (1-50): 1, preferably (2-30): 1, (5-20): 1, (8-20): 1, (10-20): 1；
In the inventive solutions, wherein step (2) it is obtained oil mutually and step (3) obtained outer aqueous phase
Volume ratio is (1-50): 1, preferably (2-30): 1, (5-20): 1, (8-20): 1, (10-20): 1；
In the inventive solutions, wherein the mass percentage of emulsifier is 1-10%, preferably 2-8%, 2-
5%；
In the inventive solutions, wherein the mass percentage of thickener is 1-10%, preferably 2-8%, 2-
5%；
In the inventive solutions, wherein the mass percentage of the stabilizer is 1-10%, preferably 2-
8%, 2-5%.
According to the technique and scheme of the present invention, at least produce it is following the utility model has the advantages that
1. technical solution of the present invention, on the one hand will effect by compounding cyprodinil to form microcapsule formulations with epoxiconazole
Unexpected technical effect is produced after the different two kinds of farm chemical ingredients compounding of mechanism, discovery has wheat sharp eyespot aobvious
The synergistic effect of work,
2. technical solution of the present invention improves drugloading rate by forming microcapsule formulations, the validity of drug ensure that.
Specific embodiment
Embodiment 1
(1) at room temperature, cyprodinil is dispersed in water, cyprodinil suspension is obtained, as inner aqueous phase；Institute
The mass percent of cyprodinil in the suspension for the inner aqueous phase cyprodinil stated is 5%；
(2) at room temperature, epoxiconazole, stabilizer are dispersed in water, obtain epoxiconazole suspension, as outer water
Phase；The mass percentage of epoxiconazole in the suspension of the outer aqueous phase epoxiconazole is 5%；
(3) at room temperature, degradable high polymer material is dissolved in toluene, obtains degradable high polymer material
Organic solvent is as oily phase；
(4) at room temperature, step (1) obtained inner aqueous phase and step (3) obtained oil are mixed, ultrasound
Obtain Water-In-Oil primary emulsion；Wherein the oil is mutually and the volume ratio of inner aqueous phase is 5:1, and the ultrasonic power is 5000W,
Ultrasonic time is 30 seconds；Ultrasonic temperature is 25 DEG C；
(5) at room temperature, that the obtained Water-In-Oil primary emulsion of step (4) is added to step (3) is obtained
In outer aqueous phase, emulsified to obtain water-oil-water type three-phase composite lotion, the Water-In-Oil primary emulsion by shaking table vibration
Volume ratio with foreign minister's water is 5:1, and the time of vibration is 30min, and temperature is 25 DEG C；
(6) water-oil-water type three-phase composite lotion that step (5) obtains is stirred, is centrifuged, washes and dries, obtains
The microcapsule formulations composition, wherein drying temperature is 50 DEG C.
Embodiment 2
(1) at room temperature, cyprodinil is dispersed in water, cyprodinil suspension is obtained, as inner aqueous phase；Institute
The mass percent of cyprodinil in the suspension for the inner aqueous phase cyprodinil stated is 8%；
(2) at room temperature, epoxiconazole, stabilizer are dispersed in water, obtain epoxiconazole suspension, as outer water
Phase；The mass percentage of epoxiconazole in the suspension of the outer aqueous phase epoxiconazole is 8%；
(3) at room temperature, degradable high polymer material is dissolved in toluene, obtains degradable high polymer material
Organic solvent is as oily phase；
(4) at room temperature, step (1) obtained inner aqueous phase and step (3) obtained oil are mixed, ultrasound
Obtain Water-In-Oil primary emulsion；Wherein the oil is mutually and the volume ratio of inner aqueous phase is 10:1, and the ultrasonic power is
5000W, ultrasonic time are 30 seconds；Ultrasonic temperature is 25 DEG C；
(5) at room temperature, that the obtained Water-In-Oil primary emulsion of step (4) is added to step (3) is obtained
In outer aqueous phase, emulsified to obtain water-oil-water type three-phase composite lotion, the Water-In-Oil primary emulsion by shaking table vibration
Volume ratio with foreign minister's water is 10:1, and the time of vibration is 30min, and temperature is 25 DEG C；
(6) water-oil-water type three-phase composite lotion that step (5) obtains is stirred, is centrifuged, washes and dries, obtains
The microcapsule formulations composition, wherein drying temperature is 50 DEG C.
Embodiment 3
The test of microcapsule formulations composition of the invention in wheat sharp eyespot pharmacodynamic test
According to the 108th part bactericidal agent for preventing and treating wheat of GBT17980.108-2004 pesticide field efficacy medicine test criterion (two)
Line disease uses the preparation-obtained microcapsule formulations composition of Example 1 and Example 2 of the present invention in wheat sharp eyespot early period of origination
It is watered spray to control, prevents and treats result and the wheat yield of current year is as shown in table 1:
Table 1: microcapsule formulations of the invention prevent and treat wheat sharp eyespot test result:
From the results shown in Table 1, using the embodiment of the present invention 1 and the microcapsule formulations of embodiment 2 in prevention and treatment wheat
Beneficial effect is produced in banded sclerotial blight test, effective to wheat increase yield, composition is promoted than single use significant effect, and
There is better slow release effect using the suspension that microcapsule formulations of the invention are compounded relative to the two.
Claims (10)
1. a kind of microcapsule formulations composition, includes following components: the suspension for containing cyprodinil as inner aqueous phase, contain fluorine
The suspension of ring azoles as outer aqueous phase, contain the oily phase of degradable high polymer material organic solvent, emulsifier, thickener, water.
2. microcapsule formulations composition as described in claim 1, which is characterized in that the suspension of the inner aqueous phase cyprodinil
In cyprodinil mass percent be 1-20%.
3. microcapsule formulations composition as described in claim 1, which is characterized in that in the suspension of the outer aqueous phase epoxiconazole
Epoxiconazole mass percentage be 1%-20%.
4. microcapsule formulations composition as described in claim 1, which is characterized in that the degradable high polymer material is selected from acyl
Change chitosan, Glycerolchitosan, poly- (lactide-caprolactone) copolymer, polyglycolide, polylactic acid, poly- (the own poly- second of lactide-
Glycol ethers) in copolymer any one or combinations thereof, wherein the mass percentage of the degradable high polymer material is
1-10%.
5. microcapsule formulations composition as described in claim 1, which is characterized in that the organic solvent is selected from dimethylbenzene, first
Benzene, ethyl alcohol, in cyclohexanone any one or combinations thereof.
6. microcapsule formulations composition pesticide according to any one of claims 1-4, which is characterized in that the emulsifier is selected from
Amphiphilic polymer, preferably polyethylene glycol monomethyl ether-polylactic acid-glycolic, polyethylene glycol, Tween-80, one in polysorbate65
Kind or any combination thereof object, wherein the mass percentage of emulsifier is 1-10%.
7. microcapsule formulations composition as described in claim 1, which is characterized in that the thickener is selected from carboxymethyl cellulose
One of element, Sodium Polyacrylate, polyacrylate or any combination thereof, wherein the mass percentage of thickener is 1-
10%.
8. microcapsule formulations composition as described in claim 1, which is characterized in that it further include stabilizer in outer aqueous phase, wherein institute
The stabilizer stated is selected from one of polyvinyl alcohol, polyvinylpyrrolidone or combinations thereof, wherein the quality of the stabilizer
Percentage composition is 1-10%.
9. the preparation method of microcapsule formulations composition as described in claim 1, it is characterised in that include the following steps:
(1) cyprodinil is dispersed in water, cyprodinil suspension is obtained, as inner aqueous phase；
(2) epoxiconazole, stabilizer are dispersed in water, epoxiconazole suspension are obtained, as outer aqueous phase；
(3) degradable high polymer material is dissolved in organic solvent, obtains the organic solvent conduct of degradable high polymer material
Oily phase；
(4) step (1) obtained inner aqueous phase and step (3) obtained oil are mixed, ultrasound obtains the primary cream of Water-In-Oil
Liquid；
(5) the obtained Water-In-Oil primary emulsion of step (4) is added in step (3) obtained outer aqueous phase, passes through shaking table
Vibration is emulsified to obtain the water-oil-water type three-phase composite lotion；
(6) water-oil-water type three-phase composite lotion that step (5) obtains be stirred, be centrifuged, washed, be dried to obtain it is described
Microcapsule formulations composition.
10. the preparation method of microcapsule formulations composition as claimed in claim 9, it is characterised in that include the following steps:
(1) cyprodinil is dispersed in water, cyprodinil suspension is obtained, as inner aqueous phase；The phonetic collarium of the inner aqueous phase
The mass percent of cyprodinil in the suspension of amine is 1-20%；
(2) epoxiconazole, stabilizer are dispersed in water, epoxiconazole suspension are obtained, as outer aqueous phase；The outer aqueous phase fluorine ring
The mass percentage of epoxiconazole in the suspension of azoles is 1%-20%；
(3) degradable high polymer material is dissolved in organic solvent, obtains the organic solvent conduct of degradable high polymer material
Oily phase；
(4) step (1) obtained inner aqueous phase and step (3) obtained oil are mixed, ultrasound obtains the primary cream of Water-In-Oil
Liquid；Wherein the oil is mutually and the volume ratio of inner aqueous phase is (1-20): (1-50), and the ultrasonic power is 100-5000W, is surpassed
The sound time is 10-30 seconds；Ultrasonic temperature is 25-50 DEG C；
(5) the obtained Water-In-Oil primary emulsion of step (4) is added in step (3) obtained outer aqueous phase, passes through shaking table
Vibration is emulsified to obtain water-oil-water type three-phase composite lotion, the body of the Water-In-Oil primary emulsion and foreign minister's water
Product is than being (1-10): (1-50), and the time of vibration is 20-60min, and temperature is 25-50 DEG C；
(6) water-oil-water type three-phase composite lotion that step (5) obtains is stirred, is centrifuged, washes and dries, obtained described
Microcapsule formulations composition, wherein drying temperature be 40-60 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101617664A (en) * | 2009-07-07 | 2010-01-06 | 陕西蒲城县美邦农药有限责任公司 | Sterilization composite containing cyprodinil and epoxiconazole |
| CN103153050A (en) * | 2009-12-15 | 2013-06-12 | Fmc有限公司 | Sustained-release silica microcapsules |
| CN103338640A (en) * | 2011-01-28 | 2013-10-02 | 迪帕克·普兰吉万达斯·沙阿 | Pesticidal composition comprising sulphur, a fungicide and an agrochemical excipient |
| CN106561644A (en) * | 2016-11-09 | 2017-04-19 | 中国科学院化学研究所 | Capsule type compound pesticide formulation and preparation method and application thereof |
-
2019
- 2019-08-13 CN CN201910743469.7A patent/CN110367250A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101617664A (en) * | 2009-07-07 | 2010-01-06 | 陕西蒲城县美邦农药有限责任公司 | Sterilization composite containing cyprodinil and epoxiconazole |
| CN103153050A (en) * | 2009-12-15 | 2013-06-12 | Fmc有限公司 | Sustained-release silica microcapsules |
| CN103338640A (en) * | 2011-01-28 | 2013-10-02 | 迪帕克·普兰吉万达斯·沙阿 | Pesticidal composition comprising sulphur, a fungicide and an agrochemical excipient |
| CN105994361A (en) * | 2011-01-28 | 2016-10-12 | 迪帕克·普兰吉万达斯·沙阿 | Pesticidal composition comprising sulphur, a fungicide and an agrochemical excipient |
| CN106561644A (en) * | 2016-11-09 | 2017-04-19 | 中国科学院化学研究所 | Capsule type compound pesticide formulation and preparation method and application thereof |
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