CN102986717A - Production method of highly efficient oil suspending agent containing acetamiprid and bifenthrin - Google Patents

Abstract

The invention relates to a production method of a highly efficient oil suspending agent containing acetamiprid and bifenthrin. The method comprises the steps of mixing, ball milling and sanding. The invention solves the problem that the acetamiprid and bifenthrin insecticide in the prior art is poor in stability and low in content when serving as an emulsifiable concentrate, and is low in pesticide efficacy when serving as a water suspending agent. The technical key point of the invention is as follows: the acetamiprid and the pyrethroid are mixed with a suitable wetting dispersant, penetrant, vegetable oil and the like, and the mixture is subjected to mixing and sanding, so that the mixture is uniformly dispersed in an oil phase to prepare a high-concentration oil-based pesticide preparation. The oil suspending agent is small in dosage, can save a large amount of packing materials, and can significantly improve the pesticide efficacy and reduce the harm to a pesticide user.

Description

The production method that contains the high efficient oil suspending agent of Acetamiprid and Biphenthrin

 

Technical field

The invention belongs to the insecticide that contains heterocyclic compound and the insecticide technical field of chrysanthemum ester class, be specifically related to a kind of production method that contains the high efficient oil suspending agent of Acetamiprid and Biphenthrin.

Background technology

Biphenthrin (bifenthrin), chemical name: 2-methyl biphenyl-3-ylmethyl-(Z)-(1RS)-and suitable-3-(2-chloro-3,3,3-three fluoro-1-acrylic)-2,2-dimethyl cyclopropane carboxylic acid ester; Biphenthrin has another name called the spirit of Uranus, worm mite, take off that mite reaches, bifenthrin, Bi Fenning etc.It is a kind of efficient pyrethroid Insecticidal and acaricidal agent.Have tag, stomach poison function, without interior suction, fumigation action.Insecticidal spectrum is wide, and mite is also had favorable effect, and effect rapidly.Not mobile in soil, safer to environment, the longevity of residure is long.The efficient synthetic pyrethroid class Insecticidal and acaricidal agent that early 1980s appears on the market.Belong to moderate toxicity.The sterling Biphenthrin is light brown solid, dissolves in chloroform, carrene, ether, toluene.Stable to light, also more stable in acid medium, but in alkaline medium, can decompose.Be mainly used in preventing and treating each Species of Lepidopterous Larvae, aleyrodid, aphid, phytophagy tetranychid.Biphenthrin is to aquatiles such as fish, and silkworm is high malicious.

Acetamiprid (acetamiprid), chemical name: N-(N-cyano group-ethyleneimine base)-N-methyl-2-chloropyridine-5-methylamine; Acetamiprid belongs to the Nitromethylene heterocycle compound, it is a kind of novel pesticide, act on the nAChR at insect nerve system cynapse position, the neural stimulation conduction of interference insect, cause the nervous system path blockade, cause neurotransmitter acetylcholine in the accumulation at cynapse position, thereby cause the insect paralysis, final dead.Have tag, stomach toxicity and stronger osmosis, desinsection is quick-acting, consumption is few, activity is high, insecticidal spectrum is wide, the lasting period reaches about 20 days, and is good etc. to Environmental compatibility.Because its mechanism of action is different from common insecticides, so the insect of organic phosphor, carbamates and pyrethroid generation resistance is had special efficacy.

Pesticide oil suspension floats agent (oil-based suspension, OD) for being insoluble to solid pesticide or the dispersion of immiscible liquids agricultural chemicals in dispersion medium of dispersion medium, consider from the production angle, the former medicine of General Requirements is solid at room temperature, and the solvability in dispersion medium (20 ℃～40 ℃ time) is lower than the pesticide species of 100mg/L.The advantage of agricultural chemicals suspension agent is evenly to mix dispersion with arbitrary proportion with dispersion medium, is subjected to the impact of dispersion medium matter little, easy to use, is difficult for contaminated environment, can directly or after the dilution spray.Preparation for processing can be made by wet pulverizing the suspension of high dispersive, continuous phase, and the average grain diameter of its particle has improved the suspensibility of particle in dispersion medium greatly generally below 3 microns, has strengthened the absorption of crops to medicament.

Present Acetamiprid and Biphenthrin preparation are the microemulsion of low content missible oil or low content and solid dosage forms and the aqueous suspension agent of part high-load.Because Acetamiprid is water-soluble stronger, generally makes the missible oil of low content or content and be lower than 30% soluble liquid and the solid dosage forms of high-load; Biphenthrin is because its low melting point and be soluble in conventional solvent xylene etc. and make conventional missible oil, microemulsion and aqueous emulsion.Composite missible oil, microemulsion and the solid pharmaceutical preparation that can only make low content of the two, and content generally is no more than 20%; Its weak point is: 1) wherein solvent is organic solvent, for example: toluene, dimethylbenzene, methyl alcohol, ethanol, isopropyl alcohol, the third reward, hexamethylene a heatable brick bed, dimethyl sulfoxide (DMSO), cyclohexanone, using has larger pollution to environment; 2) effective component content low (being generally 5～15% during use) causes serious waste to packing material, gives to produce and store and transport and brings a lot of inconvenience, aqueous suspension agent drug effect than missible oil weak effect.

Summary of the invention

The present invention is directed to problems of the prior art, purpose is to provide a kind of production method that contains the high efficient oil suspending agent of Acetamiprid and Biphenthrin oil, under the prerequisite that guarantees drug effect, can effectively reduce environmental pollution and save packing material and production and use cost.

The technical solution used in the present invention is: a kind of production method that contains the efficient suspending agent of Acetamiprid and Biphenthrin oil comprises the steps:

Step 1: add the former medicine of Acetamiprid and Biphenthrin, wetting dispersing agent, bleeding agent and vegetable oil in mixing kettle, stirring fully mixes material; The percentage by weight of each component is as follows:

Acetamiprid 1～30

Biphenthrin 1～30

Wetting dispersing agent 1～5

Bleeding agent 0.5～10

Surplus is vegetable oil;

Step 2: above-mentioned material is squeezed into ball mill, and ball milling is to the visible bulk particle of nothing;

Step 3: the material that ball milling is good is squeezed into sand milling in the sand mill again, and making its particle diameter is 2～3 microns;

Described wetting dispersing agent is one or more in alkylphenol polyoxyethylene, phenethyl phenol polyethenoxy ether, alkyl phenol formaldehyde resin polyoxyethylene ether, alkylaryl polyoxyethylene poly-oxygen propylene aether, alkylphenol polyoxyethylene sulfosuccinate, aliphatic alcohol polyoxyvinethene phosphate and the polyoxyethylene nonylphenol ether phosphate;

Described bleeding agent is fatty alcohol-polyoxyethylene ether, and title that can penetrating agent JFC is buied from Shanghai Tiantan Accessory Ingredient Co., Ltd.

Described vegetable oil comprises corn oil, soybean oil, methyl oleate, castor oil, rapeseed oil, can be one or more.

All raw materials that the present invention adopts are the commercial goods.

Wetting dispersing agent has good wetting action to dispersed pesticide activity component particle external surface, plays the effect of being convenient to disperse; Wetting dispersing agent can suppress oil-suspending agent in use flocculation and the cohesion of pesticide activity component simultaneously, plays stable effect.Bleeding agent can help oil-suspending agent to be penetrated in the water, reaches to use fast purpose; Do not contain organic solvent in the dispersion medium, but adopt vegetable oil, reduced environmental pollution.　

Production method of the present invention comprises mixing, ball milling, sand milling step, at first mixing of materials stirred, and then the grinding of process ball mill and sand mill, improved efficient.Increased the interparticle spacing of active ingredient by blend step, be conducive to wetting; By ball milling, effectively reduced the size of particle; The adding of the suitable adjuvants such as wetting dispersing agent has reduced the liquid-solid contact angle, has strengthened intergranular lubrication in the sand grinding process.

The active constituent content of conventional cream preparation generally is no more than 20%, common content is 1%～10%, the mu consumption is between 20～30ml, and take active constituent content as 40% Acetamiprid of the present invention and the Biphenthrin oil-suspending agent as example, satisfying the same medicine area, reach under the prerequisite of identical drug effect, the mu consumption is 2～3ml, can save a large amount of packing materials and cost of transportation and storage space by the improvement of formulation.Pesticides packaging thing major part is polyester bottles, supposes that an agricultural chemicals enterprise annual production 3% acetamiprid EC is 300 tons, and the price of a 200ml bottle is 0.7 yuan, needs altogether about 1,500,000 bottles, and total price is 1,050,000 yuan.If produce 40% Acetamiprid Biphenthrin oil-suspending agent, satisfying the same medicine area, reach under the prerequisite of identical drug effect, producing 30 tons of preparations gets final product, need like this 150,000 bottles, total price is 10.5 ten thousand yuan, just can save 94.5 ten thousand yuan by the independent Packaging Bottle of the improvement of formulation, and wherein the expense of chest, label does not count.

Do not contain organic solvent in the oil-suspending agent of the present invention fully, the substitute is environmentally safe, derive from the vegetable oil solvent in the environment.The simultaneously raising of active constituent content can be saved a large amount of packing bottle for pesticides again, reduces packing material to the pollution of environment.The plastic bottle of some pbz polymer resins second after second is embedded in the soil, is difficult for degraded under natural environment, can be residual 200～700 years, and caused chemical contamination residual to soil environment, greatly affect crop growth.Before without better processing packing object space method, the use that as far as possible reduces packing bottle for pesticide also is a good environmental protection behave.

Compared with prior art, oil-suspending agent active constituent content provided by the invention is high,, thus following beneficial effect had: 1, under the prerequisite that produces identical drug effect, using dosage is few; 2, in the situation of identical active ingredient amount of application, product drug effect of the present invention is high; 3, can save a large amount of packing materials, reduce production costs, reduce environmental pollution; 4, the employing vegetable oil is dispersion medium, can significantly reduce the harm to operator, reduces environmental pollution.

Embodiment

Further specify the present invention below by embodiment and Comparative Examples.Product, Comparative Examples and the clear water contrast of using respectively embodiment to produce prevent and treat the cabbage pieris field control effectiveness test, and weigh medicament to lethality rate and the control degree of cabbage pieris with insect population lethality and corrected mortality, and carry out significance test by the DMRT method.Select representationally, physical features is smooth, the fertility level uniformity, and the wild cabbage growth is neat, consistent, and experimental field 280 ㎡ (0.42 mu) that managerial skills are consistent are divided into into 28 and process residential quarters, experimental field cabbage caterpillar take 1～2 age as main.Embodiment, Comparative Examples and clear water contrast totally 7 processing are set, and each is processed and repeats 4 times, and district's group is arranged at random.Each is processed dose and is watered 50kg, according to conventional method, uses workers and peasants-16 type manual sprayer in cabbage leaves positive and negative even spraying.Every processing residential quarter is got 3 points, every some 0.33m at random ², investigation insect population radix before dispenser was investigated respectively the remaining borer population amount alive of each treatment region in 1 day, 3 days, 7 days after the dispenser, data with clear water spraying check plot are calculated natural mortality rate, calculate the insect population lethality with the data of other each treatment regions, and corrected mortality, be recorded in the table 1, formula is as follows.And with the analysis of DMRT method the significance of difference between each is processed.

Embodiment

Further specify the present invention below by embodiment and Comparative Examples.Product, Comparative Examples and the clear water contrast of using respectively embodiment to produce prevent and treat the cabbage pieris field control effectiveness test, and weigh medicament to lethality rate and the control degree of cabbage pieris with insect population lethality and corrected mortality, and carry out significance test by the DMRT method.Select representationally, physical features is smooth, the fertility level uniformity, and the wild cabbage growth is neat, consistent, and experimental field 320 ㎡ that managerial skills are consistent are divided into into 32 and process residential quarters, experimental field cabbage caterpillar take 1～2 age as main.Embodiment, Comparative Examples and clear water contrast totally 8 processing are set, and each is processed and repeats 4 times, and district's group is arranged at random.Each is processed dose and is watered 50kg, according to conventional method, uses workers and peasants-16 type manual sprayer in cabbage leaves positive and negative even spraying.Every processing residential quarter is got 3 points, every some 0.33m at random ², investigation insect population radix before dispenser was investigated respectively the remaining borer population amount alive of each treatment region in 1 day, 3 days, 7 days after the dispenser, data with clear water spraying check plot are calculated natural mortality rate, calculate the insect population lethality with the data of other each treatment regions, and corrected mortality, be recorded in the table, formula is as follows.And with the analysis of DMRT method the significance of difference between each is processed.

Embodiment 1

The production method of the high efficient oil suspending agent that contains Acetamiprid and Biphenthrin of present embodiment comprises the steps:

Step 1: add the former medicine of Acetamiprid and the former medicine of Biphenthrin, wetting dispersing agent, bleeding agent and vegetable oil in mixing kettle, stirring fully mixes material; The percentage by weight of each component is as follows:

Acetamiprid 3%

Biphenthrin 2%

Wetting dispersing agent 2%

Bleeding agent 1%

Surplus is dispersion medium.

Step 2: above-mentioned material is squeezed into ball mill, and ball milling is to the visible bulk particle of nothing;

Step 3: the material that ball milling is good is squeezed into sand milling in the sand mill again, and making its particle diameter is 2～3 microns.

In the present embodiment, wetting dispersing agent adopts phenethyl phenol polyethenoxy ether and two kinds of materials of alkylphenol polyoxyethylene, and wherein phenethyl phenol polyethenoxy ether content is 1%, and alkylphenol polyoxyethylene content is 1%; Bleeding agent adopts fatty alcohol-polyoxyethylene ether; Dispersion medium adopts methyl oleate.

Embodiment 2

The difference of the oil-suspending agent of present embodiment and embodiment 1 is, is made by the component of following percentage by weight:

Acetamiprid 5%

Biphenthrin 5%

Wetting dispersing agent 2.5%

Bleeding agent 2%

Surplus is dispersion medium.

In the present embodiment, wetting dispersing agent adopts alkyl phenol formaldehyde resin polyoxyethylene ether and two kinds of materials of aliphatic alcohol polyoxyvinethene phosphate, and wherein alkyl phenol formaldehyde resin polyoxyethylene ether content is 1%, and aliphatic alcohol polyoxyvinethene phosphate content is 1.5%; Bleeding agent adopts fatty alcohol-polyoxyethylene ether; Dispersion medium adopts methyl oleate.

Embodiment 3

The difference of the oil-suspending agent of present embodiment and embodiment 1 is, is made by the component of following percentage by weight:

Acetamiprid 10%

Biphenthrin 20%

Wetting dispersing agent 3%

Bleeding agent 2%

Surplus is dispersion medium.

In the present embodiment, wetting dispersing agent adopts phenethyl phenol polyethenoxy ether and two kinds of materials of polyoxyethylene nonylphenol ether phosphate, and wherein phenethyl phenol polyethenoxy ether content is 1%, and the polyoxyethylene nonylphenol ether phosphate ester content is 2%; Bleeding agent adopts fatty alcohol-polyoxyethylene ether; Dispersion medium adopts methyl oleate.

Embodiment 4

The difference of the oil-suspending agent of present embodiment and embodiment 1 is, is made by the component of following percentage by weight:

Acetamiprid 15%

Biphenthrin 25%

Wetting dispersing agent 5%

Bleeding agent 3%

Surplus is dispersion medium.

In the present embodiment, wetting dispersing agent adopts alkylaryl polyoxyethylene poly-oxygen propylene aether and two kinds of materials of polyoxyethylene nonylphenol ether phosphate, and wherein alkylaryl polyoxyethylene poly-oxygen propylene aether content is 2.5%, polyoxyethylene nonylphenol ether phosphate 2.5%; Bleeding agent adopts fatty alcohol-polyoxyethylene ether; Dispersion medium adopts methyl oleate.

Embodiment 5

The difference of the oil-suspending agent of present embodiment and embodiment 1 is, is made by the component of following percentage by weight:

Acetamiprid 20%

Biphenthrin 40%

Wetting dispersing agent 4%

Bleeding agent 3%

Surplus is dispersion medium.

In the present embodiment, wetting dispersing agent adopts alkylaryl polyoxyethylene poly-oxygen propylene aether and two kinds of materials of polyoxyethylene nonylphenol ether phosphate, and wherein alkylaryl polyoxyethylene poly-oxygen propylene aether content is 2%, polyoxyethylene nonylphenol ether phosphate 2%; Bleeding agent adopts fatty alcohol-polyoxyethylene ether; Dispersion medium adopts methyl oleate.

Comparative Examples 1

Active ingredient Acetamiprid weight content is 3% missible oil medicament, can buy by multiple commercial channel with the trade name of 3% Acetamiprid EC.

Comparative Examples 2

Active ingredient Biphenthrin weight content is 2.5% missible oil medicament, can be with 2.5% Biphenthrin EC

Trade name buy by multiple commercial channel.

1 day contrast table after table 1 dispenser

Numbering	The active ingredient weight content	Application dosage (g/acre)	Lethality (%)	Corrected mortality (%)	Significance F0.05	Significance F0.01
							Embodiment 1	5%	12	84.7	77.13	d	D
Embodiment 2	10%	6	85.6	78.48	d	D
							Embodiment 3	30%	2	88.7	83.11	c	C
Embodiment 4	40%	1.5	92.9	89.39	a	A
							Embodiment 5	60%	1	90.3	85.50	b	B
Comparative Examples 1	3%	20	80.9	71.45	e	E
							Comparative Examples 2	2.5%	24	81.4	72.20	e	E
The clear water contrast	-	-	33.1	-	-	-

3 days contrast tables after table 2 dispenser

Numbering	The active ingredient weight content	Application dosage (g/acre)	Lethality (%)	Corrected mortality (%)	Significance F0.05	Significance F0.01
							Embodiment 1	5%	12	88.6	83.99	d	C
Embodiment 2	10%	6	90.5	86.66	d	C
							Embodiment 3	30%	2	92.5	89.47	c	C
Embodiment 4	40%	1.5	98.2	97.47	a	A
							Embodiment 5	60%	1	95.6	93.82	b	B
Comparative Examples 1	3%	20	83.6	76.97	f	E
							Comparative Examples 2	2.5%	24	86.8	81.46	e	D
The clear water contrast	-	-	28.8	-	-	-

7 days contrast tables after table 3 dispenser

Numbering	The active ingredient weight content	Application dosage (g/acre)	Lethality (%)	Corrected mortality (%)	Significance F0.05	Significance F0.01
							Embodiment 1	5%	12	85.4	81.09	d	D
Embodiment 2	10%	6	86.4	82.38	d	D
							Embodiment 3	30%	2	89.6	86.53	c	C
Embodiment 4	40%	1.5	95.5	94.17	a	A
							Embodiment 5	60%	1	92.6	90.41	b	B
Comparative Examples 1	3%	20	81.1	75.52	f	E
							Comparative Examples 2	2.5%	24	82.1	76.81	e	E
The clear water contrast	-	-	22.8	-	-	-

The 1st day contrast table after table 1 dispenser

Numbering	The active ingredient weight content	Application dosage (g/acre)	Lethality (%)	Corrected mortality (%)	Significance F0.05	Significance F0.01
							Embodiment 1	2%	6	?	?	?	?
Embodiment 2	20%	3	?	?	?	?
							Embodiment 3	40%	1.5	92.9	89.13	a	A
Embodiment 4	60%	1	?	?	?	?
							Comparative Examples 1	3%	20	80.9	68.37	b	B
Comparative Examples 2	2.5%	24	81.4	76.83	b	B
							The clear water contrast	-	-	33.1	-	-	-

The 3rd day contrast table after table 2 dispenser

Numbering	The active ingredient weight content	Application dosage (g/acre)	Lethality (%)	Corrected mortality (%)	Significance F0.05	Significance F0.01
							Embodiment 1	2%	6	?	?	?	?
Embodiment 2	20%	3	?	?	?	?
							Embodiment 3	40%	1.5	98.2	96.97	a	A
Embodiment 4	60%	1	?	?	?	?
							Comparative Examples 1	3%	20	83.6	87.33	b	B
Comparative Examples 2	2.5%	24	86.8	83.50	b	B
							The clear water contrast	-	-	48.8	-	-	-

The 7th day contrast table after table 3 dispenser

Numbering	The active ingredient weight content	Application dosage (g/acre)	Lethality (%)	Corrected mortality (%)	Significance F0.05	Significance F0.01
							Embodiment 1	10%	6	?	?	?	?
Embodiment 2	20%	3	?	?	?	?
							Embodiment 3	40%	1.5	87.5	74.00	a	A
Embodiment 4	60%	1	?	?	?	?
							Comparative Examples 1	3%	20	85.1	59.07	b	B
Comparative Examples 2	2.5%	24	87.1	61.77	b	B
							The clear water contrast	-	-	62.8	-	-	-

By embodiment, Comparative Examples and clear water contrast control cabbage pieris field control effectiveness test, 1 day, 3 days, 7 days insecticidal effect behind medicine, embodiments of the invention all there were significant differences under F0.05 or F0.01 level property, drug effect all has obvious synergistic effect than Comparative Examples; Embodiments of the invention reduce than Comparative Examples amount of application simultaneously, have reduced use cost, have reduced environmental pollution.Therefore the high efficient oil suspending agent that contains Acetamiprid and Biphenthrin of the present invention is better than Comparative Examples.

Claims (1)

1. a production method that contains the efficient suspending agent of Acetamiprid and Biphenthrin oil comprises the steps:

Step 1: add the former medicine of Acetamiprid and Biphenthrin, wetting dispersing agent, bleeding agent and vegetable oil in mixing kettle, stirring fully mixes material; The percentage by weight of each component is as follows:

Acetamiprid 1～30

Biphenthrin 1～30

Wetting dispersing agent 1～5

Bleeding agent 0.5～10

Surplus is vegetable oil;

Step 2: above-mentioned material is squeezed into ball mill, and ball milling is to the visible bulk particle of nothing;

Step 3: the material that ball milling is good is squeezed into sand milling in the sand mill again, and making its particle diameter is 2～3 microns;

Described wetting dispersing agent is one or more in alkylphenol polyoxyethylene, phenethyl phenol polyethenoxy ether, alkyl phenol formaldehyde resin polyoxyethylene ether, alkylaryl polyoxyethylene poly-oxygen propylene aether, alkylphenol polyoxyethylene sulfosuccinate, aliphatic alcohol polyoxyvinethene phosphate and the polyoxyethylene nonylphenol ether phosphate;

Described bleeding agent is fatty alcohol-polyoxyethylene ether;

Described vegetable oil comprises corn oil, soybean oil, methyl oleate, castor oil, rapeseed oil, can be one or more.