CN1596653A - Insecticidal micro emulsion composition and its preparation method - Google Patents

Abstract

An insecticiding microemulsion is prepared through dissolving inmidacloprid and cypermethrin in cosolvent, sequentially adding surfactant, surfactant aid and antifreezing agent, stirring and adding clean water.

Description

A kind of compositions of emulsive insecticide agent and preparation method thereof

Technical field

The present invention relates to agricultural chemical insecticide, more particularly, the present invention relates to a kind of compositions of emulsive insecticide agent.Simultaneously, the invention still further relates to the preparation method of this compositions of emulsive insecticide agent.

Background technology

Produce abundant agricultural product for reaching from limited soil, in modern agriculture is produced, no matter be antenatal, produce in or postpartum, agricultural chemicals all is the indispensable important means of production.But along with general a large amount of use of agricultural chemicals, people are serious day by day to the worry and the worry of chemistry security.In view of the situation, the environment amenable new product development of the low toxicity of high activity even super-active, low-residual becomes the target of various countries pesticide science man pursuit and has obtained a feather in one's cap.As everyone knows, the new product of a new energy by modern pesticide screening test rule be obtained and huge fund, very long time of cost need be dropped into.Therefore, by the novel form exploitation, giving the serviceability that old product is new safely and effectively becomes one of direction of world's agricultural chemicals development.Need not or become the strongest representative of novel form less with the pesticidal preparations of organic solvent.

Generally speaking, be subjected to the influence of minority high-toxic pesticide, the public is mostly to the worry of chemistry security to be toxicity and the residual aspects that are embodied in active ingredient.Poisonous and hazardous organic solvent such as aromatic hydrocarbon in the Pesticidal products often are left in the basket easily to the harm that environment and human body may cause.Microemulsion is matrix with water, avoided or reduced aromatic hydrocarbon solvent to the pollution of environment with to the destruction of agroecological environment, improved the compatibility with environment greatly, is one of important development direction of formulations of pesticide development from now on.

Imidacloprid and cypermethrin compounded be domestic comparatively common a kind of insecticide, insects such as registration is used and anti-ly on the brassicaceous vegetable crop to be eliminated aphis, cabbage caterpillar.But the preparation of being processed all is to be the missible oil product of solvent with toluene or dimethylbenzene, although missible oil has good insecticidal effect, use also more convenient, but because it is organic molten wherein to contain the arene of a large amount of toxics, these solvents inevitably cause the contamination hazard of agricultural environment and agricultural product.

Summary of the invention

The objective of the invention is to overcome the deficiencies in the prior art, avoid in the Imidacloprid permethrin milk oil product aromatic hydrocarbon solvent to the contamination hazard of environment, providing a kind of is active ingredient with Imidacloprid and cypermethrin, under the effect of insecticides adjuvants such as cosolvent, surfactant, cosurfactant, antifreezing agent, the compositions of emulsive insecticide agent of spontaneous formation.Simultaneously, the invention provides a kind of preparation method of this compositions of emulsive insecticide agent.

Purpose of the present invention is achieved by following technical proposals.

Compositions of emulsive insecticide agent of the present invention, said composition is made up of following component by weight percentage:

Imidacloprid 1%～2%, cypermethrin 2%～10%, cosolvent 10%～30%, surfactant 8%～30%, the running water of cosurfactant 1%～15%, antifreezing agent 1%～5% and surplus.

Wherein: active ingredient is Imidacloprid and cypermethrin.Described cosolvent is selected from one or both in N, dinethylformamide (DMF), methyl-sulfoxide (DMSO), epoxychloropropane, cyclohexanone, the cyclohexane.Surfactant is selected from a kind of in anion surfactant or the non-ionic surface active agent or their mixture.Preferred surfactants is selected from a kind of in calcium dodecyl benzene sulfonate, neopelex, polyoxyethylene nonylphenol ether compound, nonyl phenol polyoxyethylene polyoxypropylene ether, alkylphenol-polyethenoxy polyoxypropylene ether block copolymers, alkylphenol polyoxyethylene formaldehyde condensation products, phenethyl phenol polyethenoxy ether, benzylphenol APEO and the commercially available agricultural commodity emulsifier or their mixture.Described cosurfactant is selected from a kind of in isopropyl alcohol, n-butanol, isoamyl alcohol or the isooctanol.Described antifreezing agent is selected from a kind of in ethylene glycol or the glycerine.

The invention provides a kind of preparation method of compositions of emulsive insecticide agent, this method comprises the step of following order:

(1) with cosolvent Imidacloprid, cypermethrin are fully dissolved;

(2) add surfactant, cosurfactant, antifreezing agent successively, fully stir and form uniform organic facies;

(3) stir adding running water down, form the microemulsion product of appearance transparent homogeneous, be required desinsection emulsifier combination.

To the operation of above step, when temperature is lower than 20 ℃,, cypermethrin and surfactant lose flowability owing to can solidifying, and for the ease of operation and very fast dissolving, can suitably heat and make easy to operately, dissolving is accelerated.Heating and temperature control between 20 ℃～65 ℃, heat time heating time so that practical operation and deciding generally heated 5～15 minutes.Products obtained therefrom is can spontaneous formation and can form the thermodynamic stable system of appearance transparent soup with water by any dilution proportion.

Compared with prior art, the present invention has following outstanding advantage:

1. microemulsion mainly is medium with water, the outward appearance homogeneous transparent, and drop is fine, and radius is generally between 0.01-0.1 μ m, and is littler than visible light wave, belongs to thermodynamic stable system, and its physical stability is better than water base property preparations such as existing suspending agent and aqueous emulsion.

2. compare with missible oil, microemulsion flash-point height can not burn or explode, production, storing and safe in utilization.

3, the particle of microemulsion is ultra tiny, and is littler than common missible oil particle, and plant and insect cell are had good penetration, the absorption ratio height, and low dosage just can be brought into play good drug effect.The stink that does not have the missible oil product during sprinkling.Because contained organic solvent is less, use the back that crop is stung evil and the minimizing of fruit tree fruit drop phenomenon.

4. use no or little organic solvent, environmental pollution is little, and the producer or user's murder by poisoning is greatly alleviated, and helps producing, the improvement of ecotope.

5. compare with the missible oil product of same amount, have drug effect raising, production and use cost and reduce characteristics such as low, packaged convenience, production be safe in utilization.

Embodiment

Be better explanation the present invention, the invention will be further described with specific embodiment, biologicall test and drug effect effect below.But they are not limitation of the invention.

Except as otherwise noted, the percentage that is adopted among the present invention is percetage by weight.

Embodiment 1

Product is formed 1. active ingredient: Imidacloprid 1%, cypermethrin 4%; 2. cosolvent: DMF 8%, cyclohexanone 15%; 3. surfactant: farming breast No. 500 5%, agricultural emulsifier NO 8%, farming breast No. 1,600 5%; 4. cosurfactant: n-butanol 3%; 5. antifreezing agent: ethylene glycol 2%, running water surplus.

Preparation method: in the reactor that band stirs, add the former powder of Imidacloprid, add DMF again, stir, treat that Imidacloprid dissolves the back fully and adds cypermethrin, cyclohexanone, stirring obtains Imidacloprid cypermethrin mixed solution, adds commercially available farming breast No. 500, No. 600, No. 1600, n-butanol then successively, ethylene glycol, stir uniform organic facies, in organic facies, add the surplus running water and under identical stirring condition, stir and promptly obtained 5% Imidacloprid cypermethrin microemulsion product in 10～30 minutes.

Embodiment 2

Repeat embodiment 1, following difference is arranged: 1. active ingredient: Imidacloprid 2%, cypermethrin 10%; 2. cosolvent: methyl-sulfoxide 6%, epoxychloropropane 10%; 3. surfactant: neopelex 5%, farming breast No. 33 10%, farming breast 16016%; 4. cosurfactant: isopropyl alcohol 4%; 5. antifreezing agent: glycerine 3%, running water surplus.

Embodiment 3～8

Preparation process is identical with embodiment 2, just surfactant is anion surfactant calcium dodecyl benzene sulfonate 5% and a kind of compound use of a kind of non-ionic surface active agent that is selected from polyoxyethylene nonylphenol ether, nonyl phenol polyoxyethylene polyoxypropylene ether, alkylphenol-polyethenoxy polyoxypropylene ether block copolymers, alkylphenol polyoxyethylene formaldehyde condensation products, phenethyl phenol polyethenoxy ether, alkylphenol polyoxyethylene phosphate, non-ionic surface active agent consumption 12%.

Embodiment 9～23

Preparation process is identical with embodiment 2, just surfactant be 5% calcium dodecyl benzene sulfonate respectively with the union base phenol polyethenoxy ether of consumption 12%, nonyl phenol polyoxyethylene polyoxypropylene ether, alkylphenol-polyethenoxy polyoxypropylene ether block copolymers, alkylphenol polyoxyethylene formaldehyde condensation products, phenethyl phenol polyethenoxy ether, six kinds of non-ionic surface active agents of alkylphenol polyoxyethylene phosphate in the composition of any two kinds of blended emulsifiers that are combined into.

Embodiment 24

Imidacloprid 1.5%, cypermethrin 6%, DMSO 10%, cyclohexanone 15%, farming breast No. 500 4%, farming breast No. 601 7%, farming breast No. 602 3%, peaceful breast No. 33 4%, isoamyl alcohol 3%, ethylene glycol 2%, running water surplus.

Preparation method: in the reactor that band stirs, add the former powder of Imidacloprid, add DMF again, stir, treat that Imidacloprid dissolves back adding cypermethrin, cyclohexanone fully, dissolve to obtain Imidacloprid cypermethrin mixed solution, add the farming breast successively then No. 500, No. 601, No. 602, rather newborn No. 33, isoamyl alcohol, ethylene glycol, stir uniform organic facies, in organic facies, add the surplus running water and under identical stirring condition, stir and promptly obtained 7.5% Imidacloprid cypermethrin microemulsion product in 10～30 minutes.

Embodiment 25

Imidacloprid 1.1%, cypermethrin 4.4%, DMF 8%, cyclohexanone 15%, farming breast No. 500 5%, farming breast No. 601 8%, farming breast No. 602 5%, peaceful breast No. 34 4%, n-butanol 3%, ethylene glycol 2%, running water surplus.

Preparation method: in the reactor that band stirs, add the former powder of Imidacloprid, add DMF again, stir, treat that Imidacloprid dissolves the back fully and adds cypermethrin, cyclohexanone, dissolving obtains Imidacloprid cypermethrin mixed solution, the farming of order adding afterwards breast No. 500, No. 601, No. 602, No. 34, peaceful breast, n-butanol, ethylene glycol, stir uniform organic facies, in organic facies, add the surplus running water and under identical stirring condition, stir and promptly obtained 5.5% Imidacloprid cypermethrin microemulsion product in 10～30 minutes.

Embodiment 26

Imidacloprid 2%, cypermethrin 8%, DMF12%, cyclohexanone 15%, farming breast No. 500 5%, farming breast No. 601 8%, farming breast No. 602 5%, peaceful breast No. 34 4%, n-butanol 3%, ethylene glycol 2%, running water surplus.

Preparation method: in the reactor that band stirs, add the former powder of Imidacloprid, add DMF again, stir, treat that Imidacloprid dissolves the back fully and adds cypermethrin, cyclohexanone, dissolving obtains Imidacloprid cypermethrin mixed solution, the farming of order adding afterwards breast No. 500, No. 601, No. 602, No. 34, peaceful breast, n-butanol, ethylene glycol, stir uniform organic facies, in organic facies, add the surplus running water and under identical stirring condition, stir and promptly obtained 5.5% Imidacloprid cypermethrin microemulsion product in 10～30 minutes.

The prepared microemulsion of the present invention reaches following quality standard

1. outward appearance is transparent even homogeneous liquid

2. active constituent content: 3-12%

3. breast is also stable: with 200 times of 342ppm standard hard water dilutions, leave standstill 30min under 30 ℃, keep pellucidity.Last no oil slick, following nothing precipitation.And can mix in any ratio with water.

4. low-temperature stability: low-temperature stability is qualified, freezing repeatedly-and melt and do not produce irreversible caking or muddiness, be not separated.

5. heat storage stability is qualified, and active ingredient is decomposed less than 5%.

6. the transparency temperature scope is-10 ℃-60 ℃.

Biologicall test embodiment: Imidacloprid cypermethrin microemulsion is to the toxicity test of cabbage aphid

Imidacloprid: cypermethrin (heavy virulence regression equation variance LC 50????LC 90The amount ratio)
	1∶0???????????????????Y＝5.1735+1.2344x??13.9325??0.2642???2.8945
0∶1???????????????????Y＝3.9455+1.0986x??14.4773??9.1283???134.6
	1∶1???????????????????Y＝3.0961+1.7701x??24.114???11.9008??63.1731
1∶2???????????????????Y＝3.1306+1.8021x??7.5124???10.8971??56.1553
	1∶3???????????????????Y＝3.0101+1.0922x??8.5465???11.1196??52.5672
1∶4???????????????????Y＝3.1654+2.0143x??13.4680??801429???35.3056
	1∶5???????????????????Y＝2.8562+1.8771x??15.5899??13.8702??66.9432

Sub-district, field effect experiment embodiment:

5% Imidacloprid cypermethrin microemulsion control brassicaceous vegetable aphid field control effectiveness test result

Concentration (doubly)	Insect density before the dispenser	Behind the medicine behind 2 days medicines behind 5 days medicines 10 days
								Insect density	Preventive effect (%)	Insect density	Preventive effect %	Insect density	Preventive effect (%)
		2000	?3127	?34	?98.91	?41	?98.69							?89	?97.15
1500	?1964							?15	?99.24	?0	?100	?48	?99.13
		1000	?4210	?17	?99.60	?0	?100							?21	?99.50

Claims (7)

1. compositions of emulsive insecticide agent, said composition is made up of following component by weight percentage: Imidacloprid 1%～2%, cypermethrin 2%～10%, cosolvent 10%～30%, surfactant 8%～30%, the running water of cosurfactant 1%～15%, antifreezing agent 1%～5% and surplus.

2. compositions of emulsive insecticide agent according to claim 1, wherein said cosolvent are selected from one or both in N, dinethylformamide (DMF), methyl-sulfoxide (DMSO), epoxychloropropane, cyclohexanone, cyclohexane, toluene, dimethylbenzene or the phenmethylol.

3. compositions of emulsive insecticide agent according to claim 1, wherein said surfactant is selected from a kind of in calcium dodecyl benzene sulfonate, neopelex, polyoxyethylene nonylphenol ether compound, nonyl phenol polyoxyethylene polyoxypropylene ether, alkylphenol-polyethenoxy polyoxypropylene ether block copolymers, alkylphenol polyoxyethylene formaldehyde condensation products, phenethyl phenol polyethenoxy ether, benzylphenol APEO and formaldehyde condensation products thereof, alkylphenol polyoxyethylene phosphate or the commercially available agricultural commodity emulsifier or their mixture.

4. compositions of emulsive insecticide agent according to claim 1, wherein said cosurfactant are selected from a kind of in isopropyl alcohol, n-butanol, isoamyl alcohol or the isooctanol.

5. compositions of emulsive insecticide agent according to claim 1, wherein said antifreezing agent are selected from a kind of in ethylene glycol or the glycerine.

6. the preparation method of the described compositions of emulsive insecticide agent of claim 1, this method comprises the step of following order:

(1) cosolvent fully dissolves Imidacloprid, cypermethrin;

(2) add surfactant, cosurfactant, antifreezing agent successively, fully stir and form uniform organic facies;

(3) stir adding running water down, form the microemulsion product of appearance transparent homogeneous, be required desinsection emulsifier combination.

7. the preparation method of compositions of emulsive insecticide agent according to claim 6 further is included in temperature when being lower than 20 ℃, under 20 ℃～65 ℃, with 5～15 minutes heat time heating times of gains of step (3).