CN1792162A - Micro-capsule water suspending agent for killing tick - Google Patents
Micro-capsule water suspending agent for killing tick Download PDFInfo
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- CN1792162A CN1792162A CN 200510131187 CN200510131187A CN1792162A CN 1792162 A CN1792162 A CN 1792162A CN 200510131187 CN200510131187 CN 200510131187 CN 200510131187 A CN200510131187 A CN 200510131187A CN 1792162 A CN1792162 A CN 1792162A
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Abstract
A microcapsule suspension of chlorpyrifos-ethyl is proportionally prepared from chlorpyrifos-ethyl, core solvent, protective colloid, wall material (urea and formaldehyde), wettable disperser, viscosity regulator and water through pre-polymerizing of urea and formaldehyde, depositing on the surface of core while polymerizing, solidifying and preparing microcapsule suspension. It has low poison and high and durable effect.
Description
(1) technical field
The invention belongs to formulations of pesticide manufacture field, concrete relates to be core, to be that cyst material coats the formation microcapsules with the urea-formaldehyde resin with the organophosphorus insecticide chlopyrifos, and further makes the pesticides new formulation and the technology of preparing of microcapsules aqueous suspension agent.
(2) background technology
Chlopyrifos (chlorpyrifos) is the broad-spectrum organic insecticide that substitutes the contour malicious agricultural chemicals of acephatemet, is widely applied in the control of agricultural and sanitary insect pest.Mainly be processed into missible oil at present at home and use, in recent years, also occurred the report of chlorpyrifos aqueous emulsion, microemulsion product successively, but also there are some shortcomings in the chlopyrifos of these formulations in application:
1, after the dispenser of chlopyrifos regular dosage form, active ingredient is subjected to environmental influences such as light, moisture, decomposes comparatively fast, and the lasting period on plant leaf blade is shorter;
2, the organic solvent amount of using in the main formulation missible oil of chlopyrifos is big, easily contaminated environment and cause the wasting of resources;
3, chlopyrifos is easily decomposed in water, is processed into general moisture formulation such as aqueous emulsion, microemulsion storage decomposition soon, to having relatively high expectations of stabilizing agent, selects comparatively difficulty, has influenced its industrialization.
Compare with the conventional pesticide formulation, the characteristics of toxicity and poisoning, reduction environmental pollution are run off, alleviate in the decomposition that microcapsule formulation (microcapsule suspending agent, micro-capsule granula) has the effective rate of utilization that prolongs the lasting period, improve agricultural chemicals, avoid agricultural chemicals caused by external environment, and microcapsule formulation has become one of important development direction of formulations of pesticide processing at present.Chlopyrifos is processed into the microcapsules aqueous suspension agent is expected to address the above problem, and at present domestic also not seeing uses Lauxite to prepare the research and the application report of chlorpyrifos microcapsule agent.
(3) summary of the invention
Purpose of the present invention is intended to overcome the deficiency of above-mentioned prior art, and a kind of micro-capsule water suspending agent for killing tick novel form is provided, and solving one is that regular dosage form uses the back chlopyrifos to be subject to such environmental effects and to cause short problem of lasting period; The 2nd, the high problem of organic solvent content in the chlorpyrifos ec formulation; The 3rd, because of the easy hydrolysis of active ingredient in the storage of aqueous dosage forms such as chlorpyrifos aqueous emulsion and microemulsion is difficult for the problem of processing.
Another object of the present invention provides is convenient to micro-capsule water suspending agent for killing tick prescription and the preparation method that a kind of cost is low, be convenient to suitability for industrialized production; thereby, help the sustainable development and the agriculture environmental protection of agricultural for the control of insect in the agricultural production provides a kind of new product.
The present invention is based on for this reason following some conceive and realize, the problem of poor chemical stability will select a kind of water pocket wall material of refusing that chlopyrifos is coated when 1. solving water baseization of chlopyrifos formulation and storing, and reduces contacting of the latter and water, thus the reduction resolution ratio; 2. for the market competitiveness of raising, require cyst material cheap, be convenient to reduce the preparation cost with regular dosage form; 3. preparation technical process is simple, can carry out under normal pressure, and environmental pollution is little, is convenient to industrialization and control production cost; 4. make moisture suspending agent type after chlopyrifos being coated, reduce the consumption of organic solvent and further reduce the preparation cost; 5. formulation is identical with the regular dosage form occupation mode, as suspending agent, meets peasant's medication custom, is convenient to marketing; 6. utilize the performance of touching brokenly of microcapsules, make the microcapsules aqueous suspension agent just imitate with regular dosage form quite or lower slightly, but obviously prolong the lasting period.
For achieving the above object, it is cyst material that the present invention selects Lauxite for use, utilizes in-situ polymerization technology to prepare chlorpyrifos microcapsule, and it further is prepared into aqueous suspension agent.The prescription composition of this agent is expressed as follows in weight percentage:
Chlopyrifos 5～25%, capsule heart solvent 1～10%, protective colloid 0.3～1%, cyst material 1～5%, wetting dispersing agent 2～5%, viscosity modifier 0.1～0.5%, surplus is a water.
Capsule heart solvent is a kind of in dimethylbenzene, toluene or the benzene in the prescription, and its content changes with the variation of chlopyrifos content;
Protective colloid is selected from polyvinyl alcohol, Sodium Polyacrylate, gelatin, gum Arabic in the prescription, is preferably gum Arabic;
The cyst material that coats chlopyrifos in the prescription is a urea-formaldehyde resin, is made by polycondensation reaction with mol ratio 1: 1.5～1: 2.5 by initiation material urea and formaldehyde;
For guaranteeing the wetting and spread performance of micro-capsule water suspending agent for killing tick, the wetting dispersing agent of adding is optional from tween, polyoxyethylene nonylphenol ether, OPEO, lauryl sodium sulfate, neopelex, calcium dodecyl benzene sulfonate in the prescription;
Be to keep the physical stability of preparation in storage process, need the viscosity of the hierarchy of control, the viscosity modifier in the prescription is selected from carboxymethyl cellulose, xanthans or polyvinyl alcohol, wherein xanthans preferably.
According to above-mentioned prescription, micro-capsule water suspending agent for killing tick can adopt following preparation method to obtain:
(1) urea is dissolved in the formaldehyde, the mol ratio of urea and formaldehyde is 1: 1.5～1: 2.5, add 2～3 times of weight in the deionized water of urea and formaldehyde total amount, regulate pH to 8～9 with sodium hydroxide, be warming up to 65～70 ℃, stirring at low speed reaction 1～1.5 hour obtains the clear urea resin prepolymer aqueous solution;
(2) the former medicine of chlopyrifos fully is dissolved in an amount of capsule heart solvent, the back that stirs adds an amount of urea resin prepolymer aqueous solution, adds the protecting colloid aqueous solution, and high-speed stirred forms stable O/W emulsion;
(3) reduce rotating speed, the hydrochloric acid that adds 1M is in batches turned down the pH value of system gradually, in 40 minutes system final pH value is adjusted to 2.0～2.5, after the polymerisation 1～1.5 hour, be warming up to 45 ℃ and keep solidifying in 2.0～2.5 hours cyst wall, treat that cyst wall fully solidifies the back and adds sodium hydroxide adjusting pH value 6.5～7, add an amount of Ricinate and thickener, stir and make micro-capsule water suspending agent for killing tick.
Preparation method of the present invention carries out under normal pressure.
The micro-capsule water suspending agent for killing tick microcapsules particle diameter that the present invention obtains has the characteristics of pesticide suspension concentrate at 5～20 μ m, and can directly convert water spray and use, or along with irrigation water processing soil is prevented and treated crop pests.
The fill a prescription content of death by poisoning tick of the present invention changes between 5～25%, mainly is according to its purposes, if foliar spray can be prepared into the high-load preparation, can be prepared into the low content preparation if carry out soil treatment.
Micro-capsule water suspending agent for killing tick of the present invention is compared with existing chlopyrifos pesticides formulation and process technology, has remarkable advantages:
(1) control by the capsule skin makes the chlopyrifos rate of release controlled, obviously prolongs the control phase to insect, has improved the effective rate of utilization of agricultural chemicals;
(2) because the effect of capsule skin has reduced the rate of release in water, improved bin stability, and reduced hydrobiological acute toxicity;
(3) because initiation material urea and formaldehyde cheap, encapsulation process is simple, be easy to control, so the preparation cost is lower, has improved the market competitiveness;
(4) owing to the existence of capsule skin, improved the easy mixcibility of chlopyrifos and other agricultural chemicals, can enlarge its range of application thus;
(5) solvent load is low, and is matrix with water, and storing safety is to plant safety, little to environmental influence;
Above-mentioned part characteristics of the present invention can obtain embodying in the following embodiments.
(4) embodiment
For the present invention is described better, can further specifies by following examples, but be not limited thereto:
Embodiment one
In the there-necked flask that thermometer, agitating device are housed, add urea and formaldehyde, mol ratio is 1: 1.5, the dissolving back adds 3 times to the deionized water of formaldehyde and weight of urea, regulate pH value to 8 with sodium hydroxide, be warming up to 70 ℃, stirring at low speed reaction 1 hour promptly obtains the Lauxite prepolymer aqueous solution.
Under the normal temperature the former medicine of 20.4g 98.3% chlopyrifos is dissolved in the 5.0g toluene, the back that stirs adds the above-mentioned Lauxite prepolymer of the 15g aqueous solution, and adds the gum Arabic aqueous solution of 15g 5%, and 1500 rev/mins are stirred the stable O/W emulsion of formation; Reduce rotating speed to 700 rev/min, divides 5 crowdes of adding 1M watery hydrochloric acid regulation system pH to 2.0 in 40 minutes, polycondensation reaction 1.5 hours; Be warming up to 45 ℃ of curing cyst walls and add sodium hydroxide adjusting pH to 6.5 after 2.5 hours thereafter, add 5g Tween-20, add 1% xanthan gum solution 10g again, water reaches 100g with the system gross weight, stirs and promptly obtains 20% micro-capsule water suspending agent for killing tick.
Embodiment two
In the there-necked flask that thermometer, agitating device are housed, add urea and formaldehyde, mol ratio is 1: 2.0, the dissolving back adds 2.5 times to the deionized water of formaldehyde and weight of urea, regulate pH value to 7.5 with sodium hydroxide, be warming up to 70 ℃, stirring at low speed reaction 1.5 hours promptly obtains the Lauxite prepolymer aqueous solution.
Under the normal temperature the former medicine of 10.2g 98.3% chlopyrifos is dissolved in the 2.0g benzene, the back that stirs adds the above-mentioned Lauxite prepolymer of the 10g aqueous solution, and adds the gum Arabic aqueous solution of 10g 5%, and 1300 rev/mins are stirred the stable O/W emulsion of formation; Reduce rotating speed to 700 rev/min, divides 5 crowdes of adding 1M watery hydrochloric acid regulation system pH to 2.5 in 40 minutes, polycondensation reaction 1 hour; Thereafter be warming up to 45 ℃ of curing cyst walls and add sodium hydroxide adjusting pH to 6.8 after 2.0 hours, add 5g NP-10, add 1% xanthan gum solution 15g again, water reaches 100g with the system gross weight, stirs and promptly obtains 10% micro-capsule water suspending agent for killing tick.
Embodiment three
In the there-necked flask that thermometer, agitating device are housed, add urea and formaldehyde, mol ratio is 1: 2.5, the dissolving back adds 2 times to the deionized water of formaldehyde and weight of urea, regulate pH value to 7.5 with sodium hydroxide, be warming up to 65 ℃, stirring at low speed reaction 2.0 hours promptly obtains the Lauxite prepolymer aqueous solution.
Under the normal temperature the former medicine of 5.1g 98.3% chlopyrifos is dissolved in the 2.0g dimethylbenzene, the back that stirs adds the above-mentioned Lauxite prepolymer of the 7.5g aqueous solution, and adds the gum Arabic aqueous solution of 8.0g 5%, and 1200 rev/mins are stirred the stable O/W emulsion of formation; Reduce rotating speed to 700 rev/min, divides 5 crowdes of adding 1M watery hydrochloric acid regulation system pH to 2.5 in 40 minutes, polycondensation reaction 1 hour; Be warming up to 45 ℃ of curing cyst walls and add sodium hydroxide adjusting pH to 7.0 after 2.0 hours thereafter, add 2.5g NP-10 and 2.5g lauryl sodium sulfate, add 1% xanthan gum solution 20g again, water reaches 100g with the system gross weight, promptly obtains 5% micro-capsule water suspending agent for killing tick.
The key technical indexes of the present invention such as table 1:
Table 1 micro-capsule water suspending agent for killing tick technical indicator
| Medicament | Chlopyrifos content (%) | Outward appearance | Aqueous dispersions (200 times) | Average grain diameter (μ m) | Envelop rate (%) | Bin stability |
| Embodiment one | 20 | The white thick liquid | The white suspension | 9.5 | 98.5 | Qualified |
| Embodiment two | 10 | The white thick liquid | The white suspension | 11.3 | 99.0 | Qualified |
| Embodiment three | 5 | The white thick liquid | The white suspension | 12.5 | 99.2 | Qualified |
The micro-capsule water suspending agent for killing tick that the present invention obtains shows good virulence to the slow eye of a leek fungus gnat larva, and table 2 is to contrast in indoor virulence to this worm with chlorpyrifos ec:
Table 2 micro-capsule water suspending agent for killing tick and missible oil compare (medicine embrane method) to the virulence of the slow eye of leek fungus gnat larva
| Handle medicament | Handle fate (d) | Toxicity regression formula (Y=a+bx) | LC 50 (μg/ml) | LC 90 (μg/ml) |
| Chlorpyrifos ec | 0 8 16 32 | Y＝4.4130+1.9083x Y＝2.6226+2.2391x Y＝1.9145+1.8895x Y＝1.4063+1.8000x | 2.03 11.53 42.95 99.20 | 9.53 43.07 204.76 511.09 |
| Embodiment one | 0 8 16 32 | Y＝4.2346+1.7046x Y＝4.0718+1.6898x Y＝3.2615+2.1748x Y＝2.4520+2.1498x | 2.81 3.54 6.25 15.32 | 15.88 20.31 24.12 60.45 |
| Embodiment two | 0 8 16 32 | Y＝4.2072+1.6614x Y＝4.0619+1.5159x Y＝3.0361+2.0450x Y＝2.1287+2.1744x | 3.00 4.16 9.13 20.92 | 17.72 29.13 38.64 81.27 |
| Embodiment three | 0 8 16 32 | Y＝3.8915+2.0825x Y＝2.9676+2.5968x Y＝2.6304+2.0899x Y＝2.0995+2.1547x | 3.41 6.06 13.61 22.19 | 14.05 18.89 55.86 87.28 |
Data show prescription and method obtain according to the present invention three embodiment microcapsules aqueous suspension agents and missible oil are relatively in the table, initial virulence is lower slightly, but difference is not obvious, and along with the prolongation of time, hold and imitate virulence, show that this prescription and method can prolong the control phase of chlopyrifos to the slow eye of leek fungus gnat larva then apparently higher than chlorpyrifos ec.
Table 3 micro-capsule water suspending agent for killing tick and chlorpyrifos ec are to the field control effectiveness test of the slow eye of leek fungus gnat larva
Test site: Tai'an, Shandong. processing method: water with irrigation water and to execute
| Medicament | Dosage (ml/ mu) | Each day preventive effect (%) behind the medicine | |||
| 7 days | 14 days | 21 days | 28 days | ||
| Embodiment three | 1200 | 75.83 | 83.85 | 91.77 | 88.85 |
| Embodiment two | 600 | 83.26 | 89.21 | 94.04 | 90.88 |
| Embodiment one | 300 | 85.38 | 91.29 | 85.57 | 84.37 |
| 20% chlorpyrifos ec | 300 | 84.63 | 91.17 | 81.92 | 77.03 |
Field test results shows that also the control phase of eye fungus gnat larva obviously prolongs 7-14 days to the chlopyrifos micro-capsule aqueous suspension agent that the present invention obtains late to leek than conventional missible oil formulation.
The micro-capsule water suspending agent for killing tick that the present invention obtains has had obvious reduction to hydrobiological toxicity, and table 4 is with content micro-capsule water suspending agent for killing tick and chlorpyrifos ec to the virulence of zebra fish relatively:
Table 4 micro-capsule water suspending agent for killing tick and chlorpyrifos ec compare the toxicity of zebra fish
| Medicament | Time behind the medicine | Virulence regression equation | LC 50 (mg/L) | The relative toxicity multiple |
| 20% chlorpyrifos ec | 24h 48h 72h 96h | Y＝4.8724+4.7368X Y＝5.1725+4.4129X Y＝5.5317+4.0915X Y＝5.6879+4.1090X | 1.064 0.9139 0.7414 0.6801 | - - - - |
| Embodiment one | 24h 48h 72h 96h | Y＝-8.4870+7.5225X Y＝-6.0064+6.2691X Y＝-5.1159+5.9388X Y＝-5.8914+6.5027X | 61.9701 56.9726 50.5072 47.3038 | 58.24 62.34 68.12 69.55 |
Table 4 result shows that micro-capsule water suspending agent for killing tick can be reduced to 1/50～60 of the toxicity of the missible oil of content the toxicity of zebra fish, therefore can increase substantially hydrobiological safety.
Claims (3)
1, a kind of micro-capsule water suspending agent for killing tick is characterized in that it consists of in weight percentage: chlopyrifos 5～25%, capsule heart solvent 1～10%; protective colloid 0.3～1%, cyst material 1～5%, wetting dispersing agent 2～5%; viscosity modifier 0.1～0.5%, surplus are water.
2, according to claim 1 described a kind of micro-capsule water suspending agent for killing tick, wherein capsule heart solvent is a kind of in dimethylbenzene, toluene or the benzene.
3, according to claim 1 described a kind of micro-capsule water suspending agent for killing tick, wherein cyst material is a Lauxite, is to be to obtain by polycondensation reaction in 1: 1.5～1: 2.5 by initiation material urea and formaldehyde with mol ratio.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101305725B (en) * | 2008-07-17 | 2011-05-11 | 浙江省农业科学院 | Chlopyrifos and pymtrozine composite microcapsule suspending agent and its preparation method |
| CN102057897A (en) * | 2009-11-17 | 2011-05-18 | 联合国南通农药剂型开发中心 | Chlorpyrifos microcapsule suspension and preparation method thereof |
| CN102204529A (en) * | 2011-04-02 | 2011-10-05 | 河北三农农用化工有限公司 | Lythidathion microcapsule suspension and preparation method thereof |
| CN102239831A (en) * | 2011-05-03 | 2011-11-16 | 谭晓辉 | Lythidathion microcapsule suspending agent and preparation method |
| CN102415376A (en) * | 2011-12-23 | 2012-04-18 | 谢玄 | Chlorpyrifos-containing microcapsule granules and preparation method thereof |
| CN102487941A (en) * | 2011-12-19 | 2012-06-13 | 贵州大学 | Litsea cubeba oil microcapsule suspension and preparation method thereof |
| CN101583269B (en) * | 2006-11-23 | 2014-08-27 | 加特微胶囊有限公司 | Novel pesticide formulations containing microcapsules |
| CN104054700A (en) * | 2014-06-30 | 2014-09-24 | 河北三农农用化工有限公司 | Preparation method of fosthiazate microcapsule suspension |
| CN104381251A (en) * | 2014-10-31 | 2015-03-04 | 山东农业大学 | Pesticide microcapsule employing metal ion chelate of tannin as capsule wall and preparation method of pesticide microcapsule |
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2005
- 2005-12-30 CN CN 200510131187 patent/CN1792162A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101583269B (en) * | 2006-11-23 | 2014-08-27 | 加特微胶囊有限公司 | Novel pesticide formulations containing microcapsules |
| CN101305725B (en) * | 2008-07-17 | 2011-05-11 | 浙江省农业科学院 | Chlopyrifos and pymtrozine composite microcapsule suspending agent and its preparation method |
| CN102057897A (en) * | 2009-11-17 | 2011-05-18 | 联合国南通农药剂型开发中心 | Chlorpyrifos microcapsule suspension and preparation method thereof |
| CN102057897B (en) * | 2009-11-17 | 2013-04-24 | 联合国南通农药剂型开发中心 | Chlorpyrifos microcapsule suspension and preparation method thereof |
| CN102204529A (en) * | 2011-04-02 | 2011-10-05 | 河北三农农用化工有限公司 | Lythidathion microcapsule suspension and preparation method thereof |
| CN102239831A (en) * | 2011-05-03 | 2011-11-16 | 谭晓辉 | Lythidathion microcapsule suspending agent and preparation method |
| CN102487941A (en) * | 2011-12-19 | 2012-06-13 | 贵州大学 | Litsea cubeba oil microcapsule suspension and preparation method thereof |
| CN102415376A (en) * | 2011-12-23 | 2012-04-18 | 谢玄 | Chlorpyrifos-containing microcapsule granules and preparation method thereof |
| CN104054700A (en) * | 2014-06-30 | 2014-09-24 | 河北三农农用化工有限公司 | Preparation method of fosthiazate microcapsule suspension |
| CN104381251A (en) * | 2014-10-31 | 2015-03-04 | 山东农业大学 | Pesticide microcapsule employing metal ion chelate of tannin as capsule wall and preparation method of pesticide microcapsule |
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