CN106577736A - Chlorpyrifos micro-capsule suspending agent adopting meso-porous silicon molecular sieve as carrier and preparation method thereof - Google Patents
Chlorpyrifos micro-capsule suspending agent adopting meso-porous silicon molecular sieve as carrier and preparation method thereof Download PDFInfo
- Publication number
- CN106577736A CN106577736A CN201611230297.6A CN201611230297A CN106577736A CN 106577736 A CN106577736 A CN 106577736A CN 201611230297 A CN201611230297 A CN 201611230297A CN 106577736 A CN106577736 A CN 106577736A
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- China
- Prior art keywords
- molecular sieve
- suspending agent
- carrier
- chlorpyrifos
- chlopyrifos
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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.)
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Classifications
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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
-
- 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
- A01N25/08—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 solids as carriers or diluents
-
- 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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing heterocyclic radicals
Abstract
The invention discloses a chlorpyrifos micro-capsule suspending agent adopting a meso-porous silicon molecular sieve as a carrier and a preparation technique thereof. The chlorpyrifos micro-capsule suspending agent adopting the meso-porous silicon molecular sieve as the carrier is characterized by comprising the following raw materials such as chlorpyrifos, polypropylene carbonate, polyvinyl alcohol, polylactic acid, gelatin, silicone oil emulsion, sodium alginate, organic bentonite, a MCM-41 molecular sieve, KH550, polyacrylic acid and hydrotalcite. In the chlorpyrifos micro-capsule suspending agent adopting the meso-porous silicon molecular sieve as the carrier and the preparation technique thereof, the organic bentonite and the sodium alginate are subjected to blending modification, intercalation is achieved, hydrophobicity and the adsorption effect are improved, and the organic bentonite and biodegradable material polylactic acid are combined into a wall material, so that a medicine controlled-release microcapsule is prepared. The MCM-41 molecular sieve is modified through the KH550 and serves as the carrier, the polyacrylic acid with a negative charge serves as a functional molecule, and through electrostatic adsorption, a controlled-release system is prepared. The layered hydrotalcite serves as a main body, microencapsulation chlorpyrifos serves as a guest molecule, an intercalation material is prepared, and the chlorpyrifos micro-capsule suspending agent is prepared.
Description
Technical field
The present invention relates to pesticide field, and in particular to a kind of mesoporous silica molecular sieve is the chlopyrifos microcapsule suspending agent of carrier,
And its preparation technology.
Background technology
Chlopyrifos is widely used organophosphorus insecticide, can as the succedaneum of high-toxic pesticide, can be applicable to health and
Agricultural insect management, can effectively prevent and treat over one hundred kind of insect in the various crops such as grain, vegetable, fruit tree.Chlopyrifos abnormal flavour is big,
Relatively easy photodissociation, poisoning is also easy to produce to sensitive crop, is the pollution for improving its safety and lasting period, reducing to environment, by it
Carry out microencapsulation.
Meng Rui is in its research paper《The preparation and sustained release performance evaluation of degradable poly (propylene carbonate)-chlorpyrifos microcapsule》
In one text, with poly (propylene carbonate) (PPC) as wall material, polyvinyl alcohol (PVA) is continuous phase stabiliser, is volatilized using emulsified solvent
Method is prepared for wrapping up the degradable microcapsule of chlopyrifos, and microcapsule has obvious slowly releasing effect to chlopyrifos.Take chlopyrifos former
Medicine, PPC is dissolved in dichloromethane as organic faciess, using PVA as continuous phase, will be cut in height after continuous phase and organic mixing
The emulsified dispersion of emulsion dispersion machine is cut, is allowed to form stable O/W type emulsions, 4h is stirred under room temperature, until dichloromethane is complete
Volatilization, solidifies microcapsule, by microcapsule suspension centrifugation, with distilled water wash rear lyophilization for several times, collects micro- glue
Capsule dry sample.But it is not enough to there is sustained release performance.
Polylactic acid is a kind of high molecular polymer in the present invention, nontoxic with excellent biocompatibility, degradability
Evil；The characteristics of sodium alginate has nontoxic, inexpensive, biodegradable, good biocompatibility, organobentonite and sodium alginate
Blending and modifying, realizes intercalation, improves hydrophobicity and adsorption effect, and with Biodegradable material polylactic acid wall material is complex as, and adds
Defoamer emulsified silicone oil, is obtained the slow-release microcapsule of medicine.The features such as mesoporous silicon material has regular pore canal, high-specific surface area,
MCM-41 molecular sieves are modified as carrier with KH550, with negatively charged polyacrylic acid as functional molecular, by electrostatic
Adsorption is prepared for slow-releasing system.The body based on stratiform brucite, the chlopyrifos with micro encapsulation as guest molecule, with ethanol
For solvent, intercalation material is prepared；With polymethyl methacrylate as wall material, with polyvinyl alcohol as continuous phase, poison is obtained
Dead Tickss microcapsule suspending agent.
The content of the invention
The invention mainly solves the technical problem of providing the chlopyrifos microcapsule suspension that a kind of mesoporous silica molecular sieve is carrier
Agent and its preparation technology, the microcapsule suspending agent low toxicity made according to the technique, sustained release performance are good, biodegradable.
The technical problem to be solved is realized using following technical scheme：
Chlopyrifos 5-10, poly (propylene carbonate) 25-35, polyvinyl alcohol 15-20, polylactic acid 6-12, gelatin 5-9, emulsified silicone oil
0.1-0.3, sodium alginate 3-7, organobentonite 3-6, MCM-41 molecular sieve 4-6, KH550 1-2, polyacrylic acid 3-5, neatly
Stone 2-5, dichloromethane, ethanol, toluene, distillation appropriate amount of water.
A kind of mesoporous silica molecular sieve is the preparation method of the chlopyrifos microcapsule suspending agent of carrier, it is characterised in that by following
Step is carried out：
A. by polylactic acid 1:5-10 is dissolved in dichloromethane, polyvinyl alcohol, gelatin 1:1:50-100 is dissolved in distilled water, and both mix
High speed dispersion and emulsion 30-50s, adds emulsified silicone oil, magnetic agitation 2-3h to obtain A liquid；To in sodium alginate 1:20-30 is added and steamed
Distilled water, stirring and dissolving, 1:10-15 adds organobentonite, ethanol, ultrasonic disperse 1-2h to obtain B liquid；By A, B liquid, uniformly mixing is treated
With；
B. in MCM-41 molecular sieves 1:20-30 adds toluene, stirs lower Deca KH550, under nitrogen protection, be heated to reflux,
Stirring reaction 2-4h, after being cooled to room temperature, 1:30-40 adds polyacrylic acid, distilled water, magnetic agitation 2-3h to filter, alcohol wash water
Wash 3-5 time, be dried；
C. under nitrogen protection, by brucite 1:20-30 is dissolved in ethanol and forms in clear solution, with a, b resulting material and mix
Close, tune pH is 6-7,4-8h is reacted at 60-80 DEG C, product Jing is filtered, washing alcohol is washed 3-5 time, dry in 80-90 DEG C in an oven
Dry 2-3h；
D. by poly (propylene carbonate) 1:5-10 is dissolved in dichloromethane, adds chlopyrifos, and 60-70 DEG C of vibration shakes up, with institute in c
Material mixing and emulsifying dispersion 5-10min is obtained, is allowed to form stable O/W type emulsions, water bath with thermostatic control stirring 2-4h obtains one kind
Microcapsule suspending agent.
The reaction mechanism of the present invention is as follows：
（1）Polylactic acid is a kind of high molecular polymer, with excellent biocompatibility, degradability, nonhazardouss；Sodium alginate
The characteristics of with nontoxic, inexpensive, biodegradable, good biocompatibility, organobentonite and sodium alginate blending and modifying, it is real
Existing intercalation, improves hydrophobicity and adsorption effect, and with Biodegradable material polylactic acid wall material is complex as, and adds defoamer emulsifying silicon
Oil, is obtained the slow-release microcapsule of medicine.
（2）The features such as mesoporous silicon material has regular pore canal, high-specific surface area, is carried out with KH550 to MCM-41 molecular sieves
It is modified as carrier, with negatively charged polyacrylic acid as functional molecular, slow-releasing system is prepared for by electrostatic adsorption.
（3）The body based on stratiform brucite, the chlopyrifos with micro encapsulation, with ethanol as solvent, prepares as guest molecule
Obtain intercalation material；With polymethyl methacrylate as wall material, with polyvinyl alcohol as continuous phase, chlopyrifos microcapsule suspension is obtained
Agent.
Specific embodiment
In order that technological means, creation characteristic, reached purpose and effect that the present invention is realized are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of mesoporous silica molecular sieve is the chlopyrifos microcapsule suspending agent of carrier, is obtained by the raw material of following weight parts (g)：
Chlopyrifos 5, poly (propylene carbonate) 35, polyvinyl alcohol 15, polylactic acid 12, gelatin 9, emulsified silicone oil 0.3, sodium alginate 7 has
Machine bentonite 6, MCM-41 molecular sieves 6, KH550 2, polyacrylic acid 5, brucite 5, dichloromethane, ethanol, toluene, distilled water are fitted
Amount.
A kind of mesoporous silica molecular sieve is the preparation method of the chlopyrifos microcapsule suspending agent of carrier, it is characterised in that by following
Step is carried out：
A. by polylactic acid 1:10 are dissolved in dichloromethane, polyvinyl alcohol, gelatin 1:1:50 are dissolved in distilled water, and both mix and divide at a high speed
Scattered emulsifying 40s, adds emulsified silicone oil, magnetic agitation 2h to obtain A liquid；To in sodium alginate 1:20 addition distilled water, stirring and dissolving,
1:15 add organobentonite, ethanol, ultrasonic disperse 2h to obtain B liquid；A, B liquid is uniformly mixed into stand-by；
B. in MCM-41 molecular sieves 1:20 add toluene, lower Deca KH550 of stirring under nitrogen protection, to be heated to reflux, stir
Mix reaction 2h, after being cooled to room temperature, 1:30 add polyacrylic acid, distilled water, magnetic agitation 3h to filter, and alcohol wash water is washed 3 times, is done
It is dry；
C. under nitrogen protection, by brucite 1:25 are dissolved in ethanol and form clear solution, mix with resulting material in a, b, adjust
PH is 6-7, and 4h is reacted at 70-80 DEG C, and product Jing is filtered, washing alcohol is washed 3 times, is dried 3h in 80-90 DEG C in an oven；
D. by poly (propylene carbonate) 1:10 are dissolved in dichloromethane, add chlopyrifos, 60-70 DEG C of vibration to shake up, with gained in c
Material mixing and emulsifying disperses 10min, is allowed to form stable O/W type emulsions, and water bath with thermostatic control stirring 3h obtains a kind of microcapsule and hang
Floating agent.
Above-described embodiment prepare a kind of mesoporous silica molecular sieve for carrier chlopyrifos microcapsule suspending agent performance test results such as
Shown in lower：
Good to the Pest killing effect in farmland, 10h Mortality of insect is 100%；Had good sustained release effect, 50d's is tired under natural conditions
Product medicine realeasing rate >=80%；Lasting effect is good, killing rate >=98% of 100d after medication.
Claims (2)
1. a kind of mesoporous silica molecular sieve is the chlopyrifos microcapsule suspending agent of carrier, it is characterised in that by the raw material of following weight parts
It is obtained：
Chlopyrifos 5-10, poly (propylene carbonate) 25-35, polyvinyl alcohol 15-20, polylactic acid 6-12, gelatin 5-9, emulsified silicone oil
0.1-0.3, sodium alginate 3-7, organobentonite 3-6, MCM-41 molecular sieve 4-6, KH550 1-2, polyacrylic acid 3-5, neatly
Stone 2-5, dichloromethane, ethanol, toluene, distillation appropriate amount of water.
2. a kind of mesoporous silica molecular sieve according to claim 1 is the preparation method of the chlopyrifos microcapsule suspending agent of carrier,
Characterized in that, carrying out according to the following steps：
A. by polylactic acid 1:5-10 is dissolved in dichloromethane, polyvinyl alcohol, gelatin 1:1:50-100 is dissolved in distilled water, and both mix
High speed dispersion and emulsion 30-50s, adds emulsified silicone oil, magnetic agitation 2-3h to obtain A liquid；To in sodium alginate 1:20-30 is added and steamed
Distilled water, stirring and dissolving, 1:10-15 adds organobentonite, ethanol, ultrasonic disperse 1-2h to obtain B liquid；By A, B liquid, uniformly mixing is treated
With；
B. in MCM-41 molecular sieves 1:20-30 adds toluene, stirs lower Deca KH550, under nitrogen protection, be heated to reflux,
Stirring reaction 2-4h, after being cooled to room temperature, 1:30-40 adds polyacrylic acid, distilled water, magnetic agitation 2-3h to filter, alcohol wash water
Wash 3-5 time, be dried；
C. under nitrogen protection, by brucite 1:20-30 is dissolved in ethanol and forms in clear solution, with a, b resulting material and mix
Close, tune pH is 6-7,4-8h is reacted at 60-80 DEG C, product Jing is filtered, washing alcohol is washed 3-5 time, dry in 80-90 DEG C in an oven
Dry 2-3h；
D. by poly (propylene carbonate) 1:5-10 is dissolved in dichloromethane, adds chlopyrifos, and 60-70 DEG C of vibration shakes up, with institute in c
Material mixing and emulsifying dispersion 5-10min is obtained, is allowed to form stable O/W type emulsions, water bath with thermostatic control stirring 2-4h obtains one kind
Microcapsule suspending agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611230297.6A CN106577736A (en) | 2016-12-28 | 2016-12-28 | Chlorpyrifos micro-capsule suspending agent adopting meso-porous silicon molecular sieve as carrier and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611230297.6A CN106577736A (en) | 2016-12-28 | 2016-12-28 | Chlorpyrifos micro-capsule suspending agent adopting meso-porous silicon molecular sieve as carrier and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN106577736A true CN106577736A (en) | 2017-04-26 |
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|---|---|---|---|
| CN201611230297.6A Withdrawn CN106577736A (en) | 2016-12-28 | 2016-12-28 | Chlorpyrifos micro-capsule suspending agent adopting meso-porous silicon molecular sieve as carrier and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585991A (en) * | 2018-06-29 | 2018-09-28 | 来安县金桃生态农业有限公司 | A kind of special compound fertilizer containing modified molecular screen of winter peach |
| CN110663682A (en) * | 2019-10-30 | 2020-01-10 | 淄博职业学院 | Slow-release type double-effect pesticide and preparation method thereof |
| CN110663683A (en) * | 2019-10-30 | 2020-01-10 | 淄博职业学院 | Slow-release type weeding and sterilizing double-effect pesticide and preparation method thereof |
-
2016
- 2016-12-28 CN CN201611230297.6A patent/CN106577736A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108585991A (en) * | 2018-06-29 | 2018-09-28 | 来安县金桃生态农业有限公司 | A kind of special compound fertilizer containing modified molecular screen of winter peach |
| CN110663682A (en) * | 2019-10-30 | 2020-01-10 | 淄博职业学院 | Slow-release type double-effect pesticide and preparation method thereof |
| CN110663683A (en) * | 2019-10-30 | 2020-01-10 | 淄博职业学院 | Slow-release type weeding and sterilizing double-effect pesticide and preparation method thereof |
| CN110663683B (en) * | 2019-10-30 | 2021-06-22 | 淄博职业学院 | Slow-release type weeding and sterilizing double-effect pesticide and preparation method thereof |
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Application publication date: 20170426 |