CN106577739A - Contact-breaking type microcapsule and preparation method thereof - Google Patents
Contact-breaking type microcapsule and preparation method thereof Download PDFInfo
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- CN106577739A CN106577739A CN201610962272.9A CN201610962272A CN106577739A CN 106577739 A CN106577739 A CN 106577739A CN 201610962272 A CN201610962272 A CN 201610962272A CN 106577739 A CN106577739 A CN 106577739A
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- mircrocapsule
- contacted
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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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/26—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-nitrogen bonds
- A01N57/30—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-nitrogen bonds containing aromatic radicals
-
- 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
- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
Abstract
The invention relates to a contact-breaking type microcapsule and a preparation method thereof. The contact-breaking type microcapsule comprises a capsule wall and a capsule core wrapped in the capsule wall, and is characterized in that the capsule wall is a polymer, the capsule core is an organic solution containing imidacloprid and isofenphos-methyl, the particle size of the microcapsule is 10-30 mu m, and the microcapsule is prepared with an interfacial polymerization method. The contact-breaking type microcapsule not only has the advantages of good stability, low control cost, low environmental pollution, long duration, low contact toxicity and inhalation toxicity and the like, but also can release high-concentration active ingredients once during climbing contact or feeding of insects due to uniform thickness as well as thinness and brittleness of the capsule wall, overcomes defects that pests cannot be killed but even the resistance of the pests is increased due to insufficient release quantity of slow-release microcapsules within a short time, and greatly improves the instant efficacy. The contact-breaking type microcapsule has a good control effect on underground pests such as grubs, mole crickets, cutworm, wireworm and the like as well as pests such as aphids, plant hoppers, thrips and the like at the seedling stage, and has a wide control spectrum.
Description
Technical field
The invention belongs to the preparing technical field of pesticide, is related to a kind of touch-broken containing imidacloprid and Isofenphos methyl micro-
Capsule and preparation method thereof.
Background technology
Since the fifties in last century, microcapsule technology medicines and health protection, textile, feedstuff, food, cosmetics, spice and
The fields such as printing and dyeing are applied, and Microcapsules of Pesticides is studied from beginning in 1949, and the Pennwalt companies in the U.S. exist
Micro encapsulation parathion-methyl is proposed first within 1974, receive extensive concern in pesticide circle from this microcapsule technology.China
The research of microencapsulation of pesticide is started late, and just starts to develop in 1978, achieved with certain achievement, develops micro encapsulation
The products such as parathion, phoxim, parathion-methyl and Malathion, but the slower development in commercially producing, with state foreign minister
Than also there is a big difference.
Microcapsule is, using macromolecular material as cyst wall or cyst membrane, by chemistry, physics or physicochemical method, to incite somebody to action
Pesticidal active substance (solid, liquid or gas) as the capsule heart wraps up, formation it is a kind of with semipermeability cyst membrane
Microencapsulation.Microencapsulation of pesticide preparation has that good stability, cost accounting are low, environmental pollution is little, lasting period length, contact toxicity and
The low feature of toxicity on inhalation, with the continuous enhancing of people's environmental consciousness and safety consciousness, microencapsulation of pesticide has become domestic and international
The focus of research, is just progressively becoming a development trend of pesticides new formulation.
Contacted_breaking release mircrocapsule is one kind of microcapsule, is technology content highest in current pesticides new formulation, most opens
A kind of novel form of the prospect of sending out, also has its uniqueness in addition to having the advantages that microcapsule, i.e. its cyst material pressure-sensitive is crisp
Property strong and closed performance it is good, can insecticide climb touch or when taking food disposable release high concentration effective ingredient, compensate for slow-releasing
In the microcapsule short time, burst size deficiency not only kills not dead insect easily increases the defect of pest resistance on the contrary, substantially increases wink
Between drug effect.The insect stronger for mobility, such as Gryllotalpa, Holotrichia diomphalia Batess, wireworm, aphid etc., due to its life habit it is different,
Pests occurrence rule is intricate, and general control personnel is difficult to grasp its generation and harming rule, and as pesticide easily divides in soil
Solution is lost in, efficiency time is too short, thus the pesticide used in preventing and treating often toxicity is high, consumption is big, times for spraying frequently, to environment
It is very harmful with agricultural product security, and can Contacted_breaking release mircrocapsule have efficiently, low toxicity, low-residual the characteristics of, prevention effect shows
Write.
Imidacloprid and the insecticide that Isofenphos methyl is two kinds of different mechanisms of action.Imidacloprid is nitro-methylene-type interior suction
Insecticide, is the acting body of nicotinic acetylcholine esterase receptor, and interference pest movements nervous system makes chemical signal transmit failure,
With organophosphorus pesticide no interactions resistance, preventing and treating sucking pest is primarily adapted for use in；Isofenphos methyl, belongs to organophosphorus pesticide,
Insect is tagged and stomach poison function with stronger, can be used for the crops such as Semen Tritici aestivi, Semen arachidis hypogaeae, Semen sojae atricolor, Semen Maydiss, Radix Pachyrhizi Erosi, Radix Betae, Fructus Mali pumilae
The subterranean pest-insects such as control of grubs, Gryllotalpa, wireworm.Imidacloprid and Isofenphos methyl compounding use, can play Isofenphos methyl
In soil the advantages of lasting period length, stomach poison function of tagging strong and strong imidacloprid systemic action, to Holotrichia diomphalia Batess, Gryllotalpa, cutworm,
The insects such as the aphid in the subterranean pest-insects such as wireworm and seedling stage, plant hopper, thrips have good effect.
There are the powder or emulsifiable concentrate pesticide product of imidacloprid or Isofenphos methyl single dose in the market, application is relatively wider, but
So far still both compounding Contacted_breaking release mircrocapsules are seen at end.
The content of the invention
The technical problem to be solved is, for conventional imidacloprid or the powder or cream of Isofenphos methyl single dose
Deficiency that stability that Pesticidal products are present is poor, environmental pollution is big, the lasting period is short, cost accounting is high etc., the present invention is by selecting conjunction
The wall material and auxiliary agent of suitable Microcapsules of Pesticides, and by technology controlling and process, develops that a kind of good stability, cost accounting be low, ring
Little, the lasting period length of border pollution, contact toxicity are low, preventing and treating spectrum is wide, have lasting preventive effect concurrently and the imidacloprid and methyl of moment preventive effect are different
Willow phosphorus compounds Contacted_breaking release mircrocapsule, and provides its preparation method.
For achieving the above object, the technical solution used in the present invention is as follows：
A kind of Contacted_breaking release mircrocapsule, is made up of cyst wall and the capsule-core being rolled in cyst wall, it is characterized in that cyst wall is macromolecule
Polymer, good airproof performance, capsule-core are the organic solution containing imidacloprid and Isofenphos methyl, and capsule grain diameter is 10-30 μm.
It is a kind of to prepare the method that imidacloprid and the different willow of methyl compound phosphorus Contacted_breaking release mircrocapsule, it is characterized in that poly- using interface
It is legal, carry out according to the following steps：
(1) based on 100 parts of gross mass, will 5-10 parts imidacloprid add 3-5 part organic solvents in dissolve, then with 5-20 part first
Base isofenphos crude oil mixes, and makes core material；
(2) in a reaction vessel with variable speed stirrer, 50 parts of water and 1 part of dispersant is added, 20 DEG C of constant temperature are placed in
Stirred in water bath, rotating speed are 200 turns/min；
(3), after mixing homogeneously in the core material that 3-6 parts cyst material I is prepared with step (1), pour step (2) into
In reaction vessel, rotating speed is upgraded to 500 turns/min；
(4), after 5-10 minutes, basis of microscopic observation, after the solution of step (3) forms uniform liquid pearl, adds 1-3 part capsules
Rotating speed is kept to 200 turns/min and continues stirring, supplied 100% weight with water, use 10% acetic acid solution after 50 minutes by wall material II
Reacting liquid pH value is adjusted to 5-6, is stopped stirring, is poured out reactant, as a certain concentration Contacted_breaking release mircrocapsule.
Further, the organic solvent described in step (1) is dimethyl sulfoxide, N-Methyl pyrrolidone, dimethyl methyl acid amide
Or one or more in dichloromethane；
Further, the dispersant described in step (2) is polyoxypropylene stearic acid ether, sorbitol polyoxyethylene ether, nonyl phenol
Polyoxyethylene ether, OPEO, sodium lauryl sulphate, dodecylbenzene sodium sulfonate, calcium dodecyl benzene sulfonate,
One or more in sodium carboxymethyl cellulose, polyvinyl alcohol；
Further, the cyst material I described in step (3) be INV, the one kind in polyurethane；
Further, the cyst material II described in step (4) be TRIN, TRAN, the one kind in ethylenediamine.
The imidacloprid and Isofenphos methyl that the present invention is provided compounds Contacted_breaking release mircrocapsule and preparation method thereof, with as follows
Advantage：
(1) wall thickness is uniform, thin and fragile, can when insecticide climbs and touches or take food disposable release high concentration it is effective into
Point, compensate for the deficiency of burst size in the slow-releasing microcapsule short time and not only kill not dead insect easily increasing lacking for pest resistance on the contrary
Fall into, substantially increase moment drug effect.
(2) cyst material be high molecular polymer, good airproof performance, it is suppressed that because of light, heat, air, rainwater, soil, micro- life
Decomposition and loss that the environmental factorss such as thing and other chemical substances etc. are caused, improve the stability of medicament itself, greatly prolong
The lasting period of effective ingredient, pesticide is used for multiple times so as to be prevented effectively from, greatly reduces input amount of the pesticide to environment, it is right to mitigate
The pollution of environment, is conducive to ecology and environment.
(3) cyst wall can suppress the volatility of imidacloprid and Isofenphos methyl, shelter its original abnormal flavour, reduce imidacloprid and
The contact toxicity and toxicity on inhalation of Isofenphos methyl, mitigates its zest to people and animals and the toxicity to Fish etc..
(4) imidacloprid and Isofenphos methyl compounding use, can play Isofenphos methyl in soil lasting period length, tag
Stomach poison function is strong and the advantages of strong imidacloprid systemic action, to subterranean pest-insects such as Holotrichia diomphalia Batess, Gryllotalpa, cutworm, wireworms and
The insects such as the aphid in seedling stage, plant hopper, thrips have good effect.
Specific embodiment
The above of the present invention is described in further detail below by way of specific embodiment, but this should not be understood
Scope for above-mentioned theme of the invention is only limitted to below example.Without departing from the idea case in the present invention described above, institute
There is similar replacement and change apparent to those skilled in the art, they are considered as being included in the present invention's
In the range of.
Embodiment 1
Weigh during 10g imidacloprids add 4g dimethyl sulfoxide and dissolve, then mix with 10g Isofenphos methyl crude oil, make capsule
Heart material；50mL water and 1g sodium lauryl sulphates are added in a reactor with variable speed stirrer, 20 DEG C of constant temperature are placed in
Stirred in water bath, rotating speed are 200 turns/min；By 5g INV with mix homogeneously in above-mentioned core material after, pour in reaction vessel,
Rotating speed is upgraded to 500 turns/min；After 7 minutes, 2g TRIN are added, rotating speed is kept to into 200 turns/min and continues stirring, added after 50 minutes
Enter 18mL water, reacting liquid pH value is adjusted to 5-6 with 10% acetic acid solution, stop stirring, pour out reactant, as imidacloprid and first
The weight/mass percentage composition of base isofenphos is 20% Contacted_breaking release mircrocapsule.
Embodiment 2
Weigh during 5g imidacloprids add 3g N-Methyl pyrrolidone and dissolve, then mix with 5g Isofenphos methyl crude oil, make
Core material；50mL water and 1g NPEs are added in a reactor with variable speed stirrer, 20 DEG C are placed in
Stir in water bath with thermostatic control, rotating speed is 200 turns/min；By 3g INV with mix homogeneously in above-mentioned core material after, pour into reaction hold
In device, rotating speed is upgraded to 500 turns/min；After 5 minutes, 1g TRAN are added, rotating speed is kept to into 200 turns/min and continues to stir, 50 minutes
32mL water is added afterwards, is adjusted reacting liquid pH value to 5-6 with 10% acetic acid solution, is stopped stirring, pour out reactant, as imidacloprid
Weight/mass percentage composition with Isofenphos methyl is 10% Contacted_breaking release mircrocapsule.
Embodiment 3
Weigh during 10g imidacloprids add the 3g dichloromethane and 2g dimethyl methyl acid amides for mixing in advance and dissolve, then with 20g first
Base isofenphos crude oil mixes, and makes core material；50mL water and 1g 12 are added in a reactor with variable speed stirrer
Alkyl benzene calcium sulfonate, is placed in 20 DEG C of waters bath with thermostatic control and stirs, and rotating speed is 200 turns/min；By 6g polyurethane and above-mentioned core material
After middle mix homogeneously, pour in reaction vessel, rotating speed is upgraded to 500 turns/min；After 10 minutes, 3g TRAN are added, rotating speed is kept to
200 turns/min continues stirring, and 5mL water is added after 50 minutes, adjusts reacting liquid pH value to 5-6 with 10% acetic acid solution, stops stirring
Mix, pour out reactant, the weight/mass percentage composition of as imidacloprid and Isofenphos methyl is 30% Contacted_breaking release mircrocapsule.
Embodiment 4
Weigh during 5g imidacloprids add the 3g dichloromethane for mixing in advance and dissolve, then mix with 10g Isofenphos methyl crude oil,
Make core material；50mL water and 1g sodium carboxymethyl cellulose are added in a reactor with variable speed stirrer, 20 are placed in
Stir in DEG C water bath with thermostatic control, rotating speed is 200 turns/min；By 4g polyurethane with mix homogeneously in above-mentioned core material after, pour into anti-
In answering container, rotating speed is upgraded to 500 turns/min；After 8 minutes, 2g ethylenediamines are added, rotating speed are kept to into 200 turns/min and continue stirring,
25mL water is added after 50 minutes, reacting liquid pH value is adjusted to 5-6 with 10% acetic acid solution, is stopped stirring, pour out reactant, as
The weight/mass percentage composition of imidacloprid and Isofenphos methyl is 15% Contacted_breaking release mircrocapsule.
Embodiment 5
Field control effectiveness test
(1) test medicine
1st, embodiment 1：20% imidacloprid Isofenphos methyl Contacted_breaking release mircrocapsule；
2nd, embodiment 2：10% imidacloprid Isofenphos methyl Contacted_breaking release mircrocapsule；
3rd, embodiment 3：30% imidacloprid Isofenphos methyl Contacted_breaking release mircrocapsule；
4th, embodiment 4：15% imidacloprid Isofenphos methyl Contacted_breaking release mircrocapsule；
5th, comparative examples 1：5% imidacloprid cream；
6th, comparative examples 2：40% Isofenphos methyl cream；
7th, blank.
(2) test period：In April, 2015
(3) test site：Shandong Pingdu
(4) subjects：The insects such as Holotrichia diomphalia Batess, Gryllotalpa, cutworm, wireworm, aphid, plant hopper, thrips
(5) test method
Specifically：Test sets 7 process, and each processes three repetitions, cell random alignment, plot area 50m2.According to
Experimental plot area, the good various medicaments of precise are watered after 50 kilograms of dilutions, using knapsack sprayer to Semen arachidis hypogaeae by per mu
Field even spraying, insecticidal effect see the table below.
Field control effectiveness test result
As can be seen from the above table, imidacloprid of the invention and Isofenphos methyl compounding Contacted_breaking release mircrocapsule to Holotrichia diomphalia Batess,
The insects such as Gryllotalpa, cutworm, wireworm, aphid, plant hopper, thrips have good preventive effect, with 5% imidacloprid cream and 40% methyl
Isofenphos cream is compared, not only environmental protection, and building performance notable, has moment preventive effect and lasting preventive effect concurrently.
Claims (7)
1. a kind of Contacted_breaking release mircrocapsule, it is characterised in that：It is made up of cyst wall and the capsule-core being rolled in cyst wall, cyst wall is macromolecule
Polymer, capsule-core is the organic solution containing imidacloprid and Isofenphos methyl, and the Contacted_breaking release mircrocapsule includes cyst material I
With cyst material II, cyst material I is INV, the one kind in polyurethane, and cyst material II is TRIN, TRAN, in ethylenediamine one
Kind.
2. Contacted_breaking release mircrocapsule according to claim 1, it is characterised in that：The particle diameter of the touch-broken microcapsule is
10-30μm。
3. a kind of preparation method of Contacted_breaking release mircrocapsule, it is characterised in that adopt interfacial polymerization, carry out according to the following steps：
(1) in parts by mass, will 5-10 parts imidacloprid add 3-5 part organic solvents in dissolve, then with 5-20 part Isofenphos methyls
Crude oil mixes, and makes core material；
(2) in the reaction vessel with variable speed stirrer, 50 parts of water and 1 part of dispersant are added, is placed in 20 DEG C of waters bath with thermostatic control
Stirring, rotating speed are 200 turns/min, form Matrix Solution；
(3), after mix homogeneously the core material that 3-6 parts cyst material I is prepared with step (1), the matrix for pouring step (2) into is molten
In liquid, rotating speed is upgraded to 500 turns/min, stirs 5-10 minutes；
(4) examine under a microscope, after solution prepared by step (3) forms uniform liquid pearl, add 1-3 parts cyst material II,
Rotating speed is kept to into 200 turns/min and continues stirring 50 minutes, 100 parts of ad pond om is supplied with water, form mixed solution, use 10% second
Acid solution adjusts the pH value of mixed solution to 5-6, stops stirring, pours out reactant, as Contacted_breaking release mircrocapsule.
4. the preparation method of Contacted_breaking release mircrocapsule as claimed in claim 2, it is characterised in that：It is organic described in step (1)
Solvent is one or more in dimethyl sulfoxide, N-Methyl pyrrolidone, dimethyl methyl acid amide or dichloromethane.
5. the preparation method of Contacted_breaking release mircrocapsule as claimed in claim 2, it is characterised in that：Dispersion described in step (2)
Agent be polyoxypropylene stearic acid ether, sorbitol polyoxyethylene ether, NPE, OPEO, 12
One kind in alkyl sodium sulfate, dodecylbenzene sodium sulfonate, calcium dodecyl benzene sulfonate, sodium carboxymethyl cellulose, polyvinyl alcohol
Or it is several.
6. the preparation method of Contacted_breaking release mircrocapsule as claimed in claim 2, it is characterised in that：Cyst wall described in step (3)
Material I is INV, the one kind in polyurethane.
7. the preparation method of Contacted_breaking release mircrocapsule as claimed in claim 2, it is characterised in that：Cyst wall described in step (4)
Material II is TRIN, TRAN, the one kind in ethylenediamine.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610962272.9A CN106577739A (en) | 2016-11-04 | 2016-11-04 | Contact-breaking type microcapsule and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610962272.9A CN106577739A (en) | 2016-11-04 | 2016-11-04 | Contact-breaking type microcapsule and preparation method thereof |
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| Publication Number | Publication Date |
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| CN106577739A true CN106577739A (en) | 2017-04-26 |
Family
ID=58590522
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610962272.9A Withdrawn CN106577739A (en) | 2016-11-04 | 2016-11-04 | Contact-breaking type microcapsule and preparation method thereof |
Country Status (1)
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1256070A (en) * | 1998-12-09 | 2000-06-14 | 南京林业大学 | Touch-broken microcapsule pesticide and its preparation |
| US20040115280A1 (en) * | 2001-04-10 | 2004-06-17 | Wolfgang Podszun | Microcapsules |
| CN101453896A (en) * | 2006-06-01 | 2009-06-10 | 住化环境科学株式会社 | Microcapsule |
-
2016
- 2016-11-04 CN CN201610962272.9A patent/CN106577739A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1256070A (en) * | 1998-12-09 | 2000-06-14 | 南京林业大学 | Touch-broken microcapsule pesticide and its preparation |
| US20040115280A1 (en) * | 2001-04-10 | 2004-06-17 | Wolfgang Podszun | Microcapsules |
| CN101453896A (en) * | 2006-06-01 | 2009-06-10 | 住化环境科学株式会社 | Microcapsule |
Non-Patent Citations (2)
| Title |
|---|
| 史明武 等: ""种子处理对花生虫害控制和对花生促生长的作用"", 《江苏农业科学》 * |
| 陆一匡: ""触破式微胶囊剂(绿色威雷)的研制及应"", 《江苏农药》 * |
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