CN1473473A - Rotenone and Bt suspension concentrate and preparation method thereof - Google Patents

Abstract

Rotenone and Bt suspension concentrate is to mix rotenone crystal powder or extract containing rotenone with Bt agent, then add wetting and dispersing agent, thickener, stabilizer, defoamer, antifreeze agent, thixotropic agent, pH regulator and other additives and deionized water are ball milled in a ball mill to make a suspension. The insecticide of the invention not only has good insect control effect, but also is safe for humans, livestock, natural enemies of pests and other beneficial organisms, and avoids environmental pollution caused by a large amount of organic solvents. The preparation process is simple, the cost is low, and it is suitable for popularization and application.

Description

Rotenone and Bt suspension concentrate and preparation method thereof

                      

The invention relates to a botanical insecticide, especially a suspension containing insecticidal active substances rotenone and Bt and a preparation method thereof.

technical background

The invention prepares traditional insecticidal active substances rotenone and Bt into a suspending agent with water as a carrier, so as to have strong insecticidal activity and prevent and control resistant pests.

Rotenone is not only a highly effective insecticidal active substance recognized by the world, but also safe for the environment, humans, livestock, natural enemies of pests and other beneficial organisms, and pests are not easy to develop drug resistance. It is an "environmentally friendly" insecticidal active substance. At present, countries all over the world attach great importance to it, and have successively developed a number of rotenone insecticide varieties, of which the main dosage form is emulsifiable concentrate, which causes great pollution to the environment. Bt is a well-recognized excellent microbial insecticide. Its main dosage form is wettable powder, and there are also suspension concentrates, emulsifiable concentrates and other dosage forms. Modern pesticide dosage forms are developing towards water-based, ultra-micronized, dust-free and controlled release, among which water-based is one of the main directions for the development of pesticides. Suspension concentrates with water as a carrier can reduce the amount of organic solvents, have no dust pollution caused by wettable powders and powders, and reduce the cost of pesticide production. It has become an extremely important formulation in pesticide preparations.

Technical content

The object of the invention is to propose a method for preparing rotenone and Bt suspension concentrate.

The object of the present invention is achieved through the following technical solutions:

After rotenone crystal powder or extract containing rotenone is mixed with Bt evenly, then add wetting and dispersing agent, thickener, stabilizer, defoamer, antifreeze, thixotropic agent, penetration enhancer, pH regulator and deionization The water is mixed evenly in proportion, and ball milled in a ball mill for 2.5 to 4 hours, so that the particle diameters of rotenone and Bt are all below 4 μm.

Wherein the rotenone crystal powder or the extract containing rotenone are prepared as follows: extract plants containing rotenone (such as rotenone, edamame, thorax) with chloroform, acetone, ethyl acetate, petroleum ether, methanol, ethanol, tetrahydrofuran, benzene bean, amorpha, etc.) dry powder to obtain an extract containing rotenone; or extract the extract containing rotenone with petroleum ether, chloroform, methanol, ethyl acetate, benzene, dichloromethane, and then mix petroleum ether and chloroform Solvent, benzene, methanol, and ethanol are used for crystallization, and chloroform, ethanol, methanol, and carbon tetrachloride are used for recrystallization to obtain rotenone crystal powder. Bt is a commercially available Bt agent.

A suspending agent of rotenone and Bt is characterized in that it contains 0.1%-80% of rotenone by weight, 0.1%-80% of Bt, and the rest are auxiliary agents.

The above-mentioned rotenone and Bt suspension concentrates contain by weight:

Rotenone 0.1%～80% Bt 0.1～80%

Defoamer 1%～10% Wetting and dispersing agent 0.5%～50%

Antifreeze 0.1%～5% Thickener 0.3%～10%

pH adjuster 0.1%～5% Stabilizer 0.01%～20%

Penetration enhancer 0%～10% Thixotropic agent 0.2%～3%

Deionized water 10%～80%

The wetting and dispersing agent is: sodium lignosulfonate, calcium lignosulfonate, sodium lauryl polyoxyethylene ether sulfate, alkylnaphthalene formaldehyde condensate sulfonate, sodium dodecylbenzenesulfonate, Sodium Lauryl Sulfate, Potassium Oleate (Sodium), Alkyl Polyoxyethylene Ether Sulfonate, Alkylphenol Polyoxyethylene Ether Formaldehyde Condensate, Alkylphenol Polyoxyethylene Ether, Nonylphenol Polyoxygen Vinyl ether, polyoxyethylene polyoxypropylene ether block copolymer, pull-off powder, polyglycolic acid ester sodium salt, lauryl polyoxyethylene ether phosphate ester, alkylnaphthalene formaldehyde condensate sulfonate, One or more of sodium oleic acid methyl taurine, alkyl acid polyoxyethylene ether sulfonate, starch, gelatin, hydroxymethyl cellulose and polyvinyl alcohol.

Thickeners are: xanthan gum, heteropolysaccharide, hydroxymethyl (ethyl) cellulose, methyl cellulose, gum arabic, guar gum, sodium alginate, carrageenan, pectin, polyvinyl alcohol , bentonite, synthetic hydrated silicic acid, gypsum, acrylic polymer and magnesium aluminum silicate or one or more mixed.

The stabilizer is selected from the group consisting of: pyrogallol, butyl glycidyl ether, phenyl glycidyl ether, cresyl glycidyl ether, polyvinyl glycol diglycidyl ether, epichlorohydrin, sodium sorbate, sodium benzoate, Epoxidized Soybean Oil, Linseed Oil, Hydroquinone, Anthraquinone, Eugenol, BHA, BHT, Vitamin _B , Citric Acid, Ascorbic Acid, PABA, Parabens, Propylparaben, Pyrogallic Caprylic Acid , dihydroxybenzophenone, FB-28, castor oil, olive oil, hydroquinone, dinaphthol, 1-naphthol, salicylic acid, rosemary oil, benzoic acid and soluble starch one or more mixtures.

Penetration enhancers are: laurocapram, JFC, etc.

The defoamer is any one of silicone oil, silicones, C _10-20 saturated fatty acids, C _8-10 fatty alcohols and π-ethylhexanol.

The antifreezing agent is: one or more of ethylene glycol, glycerol, propylene glycol, polyethylene glycol, sorbitol and urea.

The pH regulator is selected from sodium hydroxide, ammonia water, acetic acid, hydrochloric acid, citric acid and phosphoric acid.

The invention provides a rotenone and Bt suspending agent with high efficiency, low toxicity and no pollution, which is not easy to produce drug resistance to the environment, human and animal safety, and pests. The preparation uses water instead of an organic solvent. It disperses rotenone and Bt uniformly in water with a particle size below 4 μm by means of a dispersant and the physical dispersion of a ball mill to form an off-white preparation. The invention has simple process and low production cost.

The present invention has the following advantages:

Rotenone and Bt are dispersed in water with fine particles, so they have: ① less dust, less environmental pollution, safe for producers, users and the environment; ② high flash point, non-combustible and non-explosive, safe for production, storage and use; ③ With water as the base, it is rich in resources, low in product cost, and easy to package; ④ After the preparation is sprayed, it is distributed on the surface of crops as fine particles, so the "instantaneous" concentration of insect feeding is high, and the insecticidal effect is good.

In order to better understand the essence of the present invention, the technical content of the present invention will be described in detail below with examples, but the content of the present invention is not limited thereto.

Embodiment one: 6.0% rotenone · Bt suspension concentrate

Rotenone 1% Bt 5%

Wetting and dispersing agent 10% Thickener 5%

Stabilizer 2% Defoamer 1%

Penetration enhancer 0.5% Antifreeze 3%

Thixotropic agent 2% pH regulator 0.8%

Add deionized water to 100%.

Rotenone and Bt are calculated by active ingredients, and other components are calculated by weight. The same below.

The preparation process is as follows: firstly mix the extract containing rotenone and Bt evenly, then add wetting and dispersing agent in proportion and stir thoroughly, then add defoamer, thickener, stabilizer, penetration enhancer, antifreeze, thixotropic agent, pH regulator and deionized water, stir evenly while adding, and ball mill in a ball mill for 2.5 to 4 hours, so that the particle sizes of rotenone and Bt are all below 4 μm.

The preparation process of the following examples is similar to this.

Embodiment two: 7.5% rotenone·Bt suspension concentrate

Rotenone 0.5% Bt 7%

Wetting and dispersing agent 1 2% Thickener 6%

Stabilizer 2% Defoamer 1%

Penetration enhancer 0.5% Antifreeze 2.5%

Thixotropic agent 1.8% pH regulator 0.8%

Add deionized water to 100%. Embodiment three: 10% rotenone·Bt suspension concentrate

Rotenone 2.3% Bt 7.7%

Wetting and dispersing agent 15% Thickener 6%

Stabilizer 1.8% Defoamer 1.5%

Penetration enhancer 0.5% Antifreeze 2.5%

Thixotropic agent 2% pH regulator 1.0%

Add deionized water to 100%. Embodiment four: 15% rotenone·Bt suspension concentrate

Rotenone 3.8% Bt 11.2%

Wetting and dispersing agent 15% Thickener 8%

Stabilizer 2% Defoamer 1%

Penetration enhancer 0.8% Antifreeze 2.8%

Thixotropic agent 2.1% pH regulator 0.8%

Add deionized water to 100%. Embodiment five: 20% rotenone·Bt suspension concentrate

Rotenone 5% Bt 15%

Wetting and dispersing agent 20% Thickener 9%

Stabilizer 2% Defoamer 1%

Penetration enhancer 0.8% Antifreeze 3%

Thixotropic agent 2.5% pH adjuster 1.0%

Add deionized water to 100%. The application effect of the present invention is as follows:

Table 1 Control effect of rotenone·Bt mixture suspension on Plutella xylostella Drug type Dilution factor Number of predrug worms Day 3 after taking medicine Day 7 after taking medicine Corrected population reduction rate % Anti-efficacy% Corrected population reduction rate % Anti-efficacy% CK 162 -8.67% -19.31% 6.0% Rotenone·Bt Suspension Concentrate 1500× 137 60.34% 59.71%ab 93.87% 92.63%ab 7.5% Rotenone·Bt Suspension Concentrate 1500× 128 62.58% 61.39%a 96.83% 94.18%a 2.5% Rotenone EC 1000× 143 56.72% 55.64%c 88.49% 87.65%cd 7.5% Kang Duohui suspension concentrate (active ingredient is Bt) 1500× 151 52.49% 51.73%d 90.16% 89.27%c Note: The same letter after the data in the same column in the table indicates that the difference is not significant at the 5% level by analysis of variance (DMRT method)

Claims (10)

1. A suspending agent of rotenone and Bt, characterized in that it contains 0.1% to 80% by weight of rotenone, 0.1% to 60% of Bt, and all the other are auxiliary agents. 2. a suspending agent of rotenone and Bt, characterized in that it contains by weight: Rotenone 0.1%～80% Bt0.1～60% Defoamer 1%～10% Wetting and dispersing agent 0.5%～50% Antifreeze 0.1%～5% Thickener 0.3%～10% pH adjuster 0.1%～5% Stabilizer 0.01%～20% Penetration enhancer 0%～10% Thixotropic agent 0.2%～3% Deionized water 10%～80% 3. rotenone and Bt suspending agent according to claim 1, it is characterized in that wetting and dispersing agent is: sodium lignosulfonate, calcium lignosulfonate, sodium lauryl polyoxyethylene ether sulfate, alkylnaphthalene formaldehyde Condensate Sulfonate, Sodium Dodecylbenzene Sulfonate, Sodium Lauryl Sulfate, Potassium Oleate (Sodium), Alkyl Polyoxyethylene Ether Sulfonate, Alkylphenol Polyoxyethylene Ether Formaldehyde Condensate , Alkylphenol polyoxyethylene ether, Nonylphenol polyoxyethylene ether, Polyoxyethylene polyoxypropylene ether block copolymer, Pull open powder, Polyglycolate sodium salt, Lauryl polyoxygen Vinyl ether phosphate, alkylnaphthalene formaldehyde condensate sulfonate, sodium oleic acid methyl amino ethyl sulfonate, alkyl acid polyoxyethylene ether sulfonate, starch, gelatin, hydroxymethylcellulose, polyethylene Any one or more of alcohols. 4. rotenone and Bt suspending agent according to claim 1, is characterized in that thickener is: xanthan gum, heteropolysaccharide, hydroxymethyl (ethyl) cellulose, methyl cellulose, gum arabic, guar beans Glue, sodium alginate, carrageenan, pectin, polyvinyl alcohol, bentonite, synthetic hydrated silicic acid, gypsum, acrylic polymer, and magnesium aluminum silicate. 5. rotenone according to claim 1 and Bt suspending agent, it is characterized in that stabilizing agent is selected from: epichlorohydrin, pyrogallol, butyl glycidyl ether, phenyl glycidyl ether, cresyl glycidyl ether, Polyethylene glycol diglycidyl ether, sodium sorbate, sodium benzoate, epoxidized soybean oil, linseed oil, hydroquinone, anthraquinone, eugenol, BHA, BHT, V _B , citric acid, ascorbic acid, PABA, Paraben, Propylparaben, Pyrogallic Caprylic Acid, Dihydroxybenzophenone, FB-28, Castor Oil, Olive Oil, Hydroquinone, Binaphthol, 1-Naphthalene One or more mixtures of phenol, salicylic acid, rosemary oil, benzoic acid, and soluble starch. 6. rotenone and Bt suspension according to claim 1 is characterized in that penetration enhancer is: laurocapram, JFC etc. 7. rotenone and Bt suspending agent according to claim 1, it is characterized in that defoamer is: silicone oil, silicones, C _10-20 saturated fatty acids, C _8-10 fatty alcohols, π-ethylhexyl any of the alcohols. 8. rotenone and Bt suspension according to claim 1 is characterized in that antifreezing agent is: one or more mixes in ethylene glycol, glycerol, propylene glycol, polyethylene glycol, sorbitol, urea. 9. rotenone and Bt suspending agent according to claim 1, is characterized in that pH regulator is: select in sodium hydroxide, ammoniacal liquor, acetic acid, hydrochloric acid, citric acid and phosphoric acid. 10. A preparation method for rotenone and Bt suspending agent, characterized in that: first the rotenone crystal powder or the extract containing rotenone are mixed with Bt in proportion, then fully stirred and mixed evenly with the wetting and dispersing agent, and then add defoaming agent successively Thickener, thickener, stabilizer, penetration enhancer, antifreeze agent, thixotropic agent, pH regulator and deionized water, stir evenly while adding, and ball mill in a ball mill for 2.5 to 4 hours to make the particle size of rotenone and Bt Serve when all are below 4μm.