CN111418600A

CN111418600A - Emamectin benzoate indoxacarb suspension emulsion and preparation method thereof

Info

Publication number: CN111418600A
Application number: CN202010315502.9A
Authority: CN
Inventors: 王蕾; 刘会涛; 王翔; 王从爱
Original assignee: Shandong Bio Biotechnology Co ltd
Current assignee: Shandong Bio Biotechnology Co ltd
Priority date: 2020-04-20
Filing date: 2020-04-20
Publication date: 2020-07-17

Abstract

The invention relates to the technical field of pesticide preparations, in particular to an emamectin benzoate indoxacarb suspending agent and a preparation method thereof, wherein the suspending agent is prepared from the following raw materials in percentage by weight: 2-7% of emamectin benzoate, 10-20% of indoxacarb, 3-10% of carrier, 1-3% of surfactant, 5-10% of organic solvent and the balance of water, wherein the carrier is a white carbon black/titanium dioxide composite material; the invention can adsorb active ingredients in the carrier, improves the stability of the suspending agent, and avoids local agglomeration or sedimentation of the active ingredients, thereby improving the drug effect of the suspending agent, and leading the suspension rate of the emamectin benzoate to reach 99.90 percent and the suspension rate of the indoxacarb to reach 99.30 percent; the control effect of the suspending agent on the rice leaf rollers after being applied for 14 days can reach 97.20 percent to the maximum extent, and the insecticidal effect is excellent.

Description

Emamectin benzoate indoxacarb suspension emulsion and preparation method thereof

Technical Field

The invention relates to the technical field of pesticide preparations, in particular to emamectin benzoate-indoxacarb suspension emulsion and a preparation method thereof.

Background

Cnaphalocrocis medinalis, also known as leaf roller, white leaf worm, bracteal, etc., is one of the main pests in rice producing areas in China and is widely distributed in various rice areas. In addition to rice damage, cnaphalocrocis medinalis can also eat crops such as barley, wheat, sugarcane, millet, and weeds such as barnyard grass, Leersia hexandra, paspalum distichum, digitaria sanguinea, green bristlegrass, cricket grass, thatch, and reed. The rice leaf rollers can damage rice when larvae grow, can be attached with leaves to form longitudinal buds, hide and eat the upper epidermis and mesophyll of rice leaves, and only leave the white lower epidermis of the rice leaves, so that the rice is damaged in the seedling stage, the normal growth of the rice is influenced, and even the rice is withered; the rice is damaged from the tillering stage to the jointing stage, the tillering is reduced, the plant is shortened, and the growth period is delayed; after booting, particularly, the sword-like leaves are damaged during heading to heading period, so that flowering and fructification are influenced, the rate of empty shells is improved, and the thousand-kernel weight is reduced.

In order to solve the harm of the rice leaf roller to the grain crops, pesticide preparations for preventing and killing the rice leaf roller are developed at present. Methylamino avermectin benzoate (emamectin benzoate), also known as Velcro, moth-resistance, hunger worm, vegetable mint and the like, is a novel high-efficiency semi-synthetic macrocyclic lactone insecticidal antibiotic obtained by taking a soil actinomycete (Streptomyces avermitilis MA-4680) fermentation product, namely avermectin B1, as a parent compound to carry out structural modification through Wilkinson reaction, and the most sensitive target in an insect body is the stimulation effect on a neurotransmitter such as a glutamine GABA inhibitory chloride ion channel, cell function loss and muscle paralysis are caused by transferring a high-affinity binding site, nerve conduction is disturbed, the insect stops feeding immediately after contacting or taking food, and irreversible paralysis and death occur. The emamectin benzoate has the characteristics of low toxicity, high efficiency, high selectivity, good environmental compatibility and the like, has incomparable activity with other pesticides for a plurality of pests, and particularly has high pesticide effect on lepidoptera and diptera, such as red-banded leafworm, tobacco aphid moth, cotton bollworm, tobacco hornworm, diamond back moth armyworm, beet armyworm, plutella xylostella, cabbage looper, cabbage caterpillar, cabbage stem borer, cabbage striped moth, potato beetle, Mexican beetle and the like; the pesticide composition is mainly applied to rice for preventing and controlling cnaphalocrocis medinalis, has insecticidal activity 1-3 orders of magnitude higher than that of a parent compound abamectin, has stomach toxicity and contact killing effects, has a good effect at a very low dose, and is safe to natural enemies. Therefore, emamectin benzoate has been widely used in pesticide formulations. Indoxacarb (indoxacarb), also known as diazole or sanda, has a unique mechanism of action, with no cross-resistance with other insecticides; the DCJW is quickly converted into DCJW (N-demethoxycarbonyl metabolite) in an insect body, acts on an inactivated state voltage-gated sodium ion channel of an insect nerve cell by the DCJW, irreversibly blocks and destroys nerve impulse transmission in the insect body, leads pests to dyskinesia, failure in feeding and paralysis and finally death; the indoxacarb can effectively prevent and control various pests on crops such as grains, cotton, fruits, vegetables and the like.

In the prior art, emamectin benzoate and indoxacarb are compounded to obtain an insecticidal pesticide suitable for rice leaf rollers. The invention patent with the publication number of CN 101595867B discloses an emamectin benzoate-indoxacarb suspoemulsion and a preparation method thereof, wherein the suspoemulsion comprises the following components in percentage by weight: 0.5-1.5% of emamectin benzoate, 2-10% of indoxacarb, 2-8% of emulsifier, 1-5% of dispersant, 0.1-1% of anti-precipitation agent, 2-10% of antifreeze agent, 0.5-2% of antioxidant, 0.5-2% of wetting agent, 1-3% of defoaming agent, 5-10% of solvent and 100% of water; the emulsifier is EO-PO block copolymer; the dispersing agent is polyoxyethylene ether phosphate; the anti-settling agent is xanthan gum; the antifreeze agent is glycol; the antioxidant is 2, 6-di-tert-butyl-p-cresol; the wetting agent is nonylphenol polyoxyethylene ether; the defoaming agent is organic silicon; the solvent is xylene. The compound agent has the effects of contact poisoning and stomach poisoning, and can effectively prevent and treat various pests on crops such as grains, cotton, fruits, vegetables and the like.

However, the above prior art has the following drawbacks: firstly, the emamectin benzoate serving as the main active ingredient is unstable to ultraviolet light and is easy to photolyze in the using process, so that the stability of the suspending agent is reduced, and the drug effect is reduced; secondly, the emamectin benzoate serving as the main active ingredient is easy to swell in water, so that the emamectin benzoate is locally agglomerated or settled in the suspending agent, the dispersion uniformity of the emamectin benzoate is influenced, and the drug effect is reduced.

Disclosure of Invention

The first purpose of the invention is to provide an emamectin benzoate-indoxacarb suspension emulsion which can adsorb active ingredients in a carrier, improve the stability of a suspension agent, avoid local agglomeration or sedimentation of the active ingredients and further improve the drug effect of the suspension agent.

The second purpose of the invention is to provide a preparation method of the emamectin benzoate-indoxacarb suspoemulsion.

The first purpose of the invention is realized by the following technical scheme:

a emamectin benzoate-indoxacarb suspension emulsion is prepared from the following raw materials in percentage by weight: 2-7% of emamectin benzoate, 10-20% of indoxacarb, 3-10% of carrier, 1-3% of surfactant, 5-10% of organic solvent and the balance of water, wherein the carrier is a white carbon black/titanium dioxide composite material.

By adopting the technical scheme, the main active ingredients of emamectin benzoate and indoxacarb can be adsorbed in the carrier by adding the carrier in the suspending agent. The carrier is a white carbon black/titanium dioxide composite material, the white carbon black has large internal and external specific surface area and strong adsorption performance, and can adsorb a large amount of water molecules in water to be swelled into superfine particles to form stable suspension; the ultraviolet-ray absorbing material has strong ultraviolet-ray reflecting capacity and good stability, and does not decompose or discolor after being irradiated by ultraviolet rays and does not react with other components. The titanium dioxide has strong ultraviolet resistance. In the invention, the composite of the white carbon black and the titanium dioxide is utilized to absorb the active ingredients in the composite while bearing the main active ingredients of emamectin benzoate and indoxacarb carrier, and the active ingredients are slowly released after application; on one hand, the composition can play a role in protecting active ingredients from ultraviolet rays, and on the other hand, the composition can prolong the exertion time of the drug effect. The surfactant is added to improve the ductility and permeability of the effective components on plant leaves, so that the drug effect of the suspending agent is improved.

Preferably, the average particle size of the white carbon black/titanium dioxide composite material is not less than 1000 meshes.

By adopting the technical scheme, the active ingredients are more favorably adsorbed by the carrier and then uniformly dispersed in the suspending agent, and the drug effect of the suspending agent is improved.

Preferably, the white carbon black/titanium dioxide composite material is prepared by the following steps:

a: performing dispersion pretreatment on white carbon black and titanium dioxide;

b: and (b) mixing the white carbon black treated in the step (a) with titanium dioxide according to the weight ratio of 1 (1-4), and carrying out superfine grinding to obtain the product.

By adopting the technical scheme, the median diameter of the white carbon black particles is about 25 mu m, the particles are thick, and the distribution range is wide because of SiO₂Due to multiple agglomeration of particles, in order to obtain the white carbon black/titanium dioxide composite material with proper particle size and excellent performance, the white carbon black/titanium dioxide composite material needs to be subjected to dispersion treatment before compounding, so that the particle size of the white carbon black/titanium dioxide composite material meets the compounding requirement. The Ti-O bond in the titanium dioxide has larger polarity, so that water adsorbed on the surface of the titanium dioxide is polarized and ionized to form hydroxyl, and the hydroxyl has certain activity and can promote titanium dioxide particles to agglomerate, so that the titanium dioxide particles need to be dispersed before compounding. According to the white carbon black/titanium dioxide composite material prepared by the method, the surface of a white carbon black particle agglomerate is uniformly coated with titanium dioxide particles, and the white carbon black and the titanium dioxide particles are mutually interpenetrated to provide a carrier support and an anti-ultraviolet protection cavity for active ingredients.

Preferably, in the step a, the white carbon black is subjected to dispersion pretreatment as follows: and (3) in the presence of sodium polyacrylate, carrying out superfine grinding on the white carbon black to obtain the white carbon black with the median diameter of 8-12 mu m.

Through adopting above-mentioned technical scheme, white carbon black's aggregate structural strength is great, and ordinary mechanical stirring and ultrasonic dispersion can not be separately the aggregate. The dispersion of the white carbon black aggregates can be better realized by carrying out superfine grinding in the presence of an organic dispersant.

Preferably, in the step a, the titanium dioxide is subjected to superfine grinding to obtain the titanium dioxide with the median diameter of 3-5 μm.

By adopting the technical scheme, compared with the white carbon black, the titanium dioxide has far lower hydroxyl number on the particle surface than the white carbon black and weaker activity than the white carbon black, so that the agglomeration among the titanium dioxide particles is relatively weaker. The dispersion of the titanium dioxide aggregate can be better realized through superfine grinding.

Preferably, the white carbon black is precipitated white carbon black, and the titanium dioxide is rutile titanium dioxide.

By adopting the technical scheme, the precipitated white carbon black has the functions of thickening, preventing sedimentation and improving storage stability in the suspending agent, and can prevent the suspending agent from being creamed. In the ultraviolet light wavelength range, the precipitated white carbon black mainly has strong reflectivity, and the rutile type titanium dioxide has strong absorptivity; both are highly reflective in the visible range. The two materials have synergistic effect, so that the ultraviolet shielding effect of the composite material is more obvious.

Preferably, the surfactant is one or more of dodecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide and didecyl dimethyl ammonium bromide.

By adopting the technical scheme, a large number of experiments show that after the one or more surfactants are added, a stable dense adsorption layer can be formed on the surface of the carrier in the suspension system, so that the active ingredients are stably adsorbed, the active ingredients are not easy to settle or agglomerate, the stability of the suspension agent is improved, and the drug effect is improved.

Preferably, the organic solvent is one or more of xylene, toluene and ethanol.

Preferably, the feed also comprises the following raw materials in percentage by weight: 0.01-0.03% of bromochlorohydantoin.

By adopting the technical scheme, the chemical name of the bromochlorohydantoin is 1-bromo-3-chloro-5, 5-dimethylhydantoin, also named dimethachlon, bromochlorodimethylhydantoin and white powder. The bromochloro sea can be dissolved in water to release bromide ions and carbanions, can form hypobromous acid and hypochlorous acid, has strong oxidizing property, and can oxidize biological enzymes in a living body. A large number of experiments show that the pesticide effect of the suspending agent on the rice leaf roller can be further enhanced by adding the bromochlorohydantoin into the suspending agent.

The second purpose of the invention is realized by the following technical scheme:

a preparation method of the emamectin benzoate-indoxacarb suspoemulsion is characterized by comprising the following steps: the raw materials are mixed and dispersed according to the weight percentage, and the emamectin benzoate-indoxacarb suspension emulsion is obtained after shearing.

In conclusion, the invention has the following beneficial effects:

(1) according to the invention, the white carbon black/titanium dioxide composite material is used as a carrier, so that the carrier adsorbs active ingredients of the suspending agent, the median diameter of particles in the suspending agent is less than 5 microns, the suspending agent has good suspending performance, the suspending rate of emamectin benzoate can reach 99.90% at most, and the suspending rate of indoxacarb can reach 99.30% at most;

(2) the suspending agent has excellent uvioresistant performance and good stability, the content of emamectin benzoate can reach 1.58 percent at most after 48 hours of ultraviolet illumination, and the decomposition rate is only 21 percent; the content of indoxacarb can reach 14.02 percent at most, and the decomposition rate is only 6.53 percent;

(3) the suspending agent disclosed by the invention has the highest prevention and treatment effect on rice leaf rollers of 97.20% after being applied for 14 days, and has an excellent insecticidal effect.

Detailed Description

The present invention will be further described with reference to the following specific examples.

The raw materials of the invention are all commercial products, and specifically comprise: the emamectin benzoate is selected from 97% of emamectin benzoate raw drug; indoxacarb is selected from concentrated in massIndoxacarb with the degree of 99 percent; the precipitated white carbon black is synthesized by an alkali dissolution-acid precipitation method for quartz sand, wherein SiO₂94.4% by mass of Na₂2.4% by mass of O, SO₃The mass content is 2.4%; the rutile titanium dioxide is selected from DuPont R902, and the sodium polyacrylate is selected from sodium polyacrylate Derin 42N.

Preparation example 1

The carrier white carbon black/titanium dioxide composite material is prepared by the following steps:

a: dispersing and pretreating white carbon black: adding sodium polyacrylate accounting for 10 percent of the total weight of the slurry under the conditions of 24 ℃, 1500r/min of rotation speed, 5:1 of ball-to-material ratio and 2.5 percent of slurry concentration, and carrying out superfine grinding for 90min to obtain the dispersed white carbon black with the median diameter of 8-12 mu m;

dispersing and pretreating titanium dioxide: carrying out superfine grinding for 60min at the conditions of 25 ℃, 1500r/min of rotation speed, 5:1 of ball-to-material ratio and 50% of slurry concentration to obtain titanium dioxide with the median diameter of 3-5 mu m after dispersion treatment;

b: and c, mixing the white carbon black treated in the step a with titanium dioxide according to the weight ratio of 1:1, controlling the slurry concentration to be 10%, carrying out superfine grinding for 35min, and sieving to obtain the white carbon black/titanium dioxide composite material with the average particle size of 1000 meshes.

Preparation example 2

The preparation steps of the white carbon black/titanium dioxide composite material of the preparation example 2 are different: b: b, mixing the white carbon black treated in the step a with titanium dioxide according to the weight ratio of 1:2.5, controlling the slurry concentration to be 10%, carrying out superfine grinding for 35min, and sieving to obtain a white carbon black/titanium dioxide composite material with the average particle size of 1000 meshes; the rest is the same as in preparation example 1.

Preparation example 3

The difference of the preparation steps of the white carbon black/titanium dioxide composite material of the preparation example 3 is that: b: b, mixing the white carbon black treated in the step a with titanium dioxide according to the weight ratio of 1:3.5, controlling the slurry concentration to be 10%, carrying out superfine grinding for 35min, and sieving to obtain a white carbon black/titanium dioxide composite material with the average particle size of 1000 meshes; the rest is the same as in preparation example 1.

Preparation example 4

The preparation steps of the white carbon black/titanium dioxide composite material of the preparation example 4 are different: b: b, mixing the white carbon black treated in the step a with titanium dioxide according to the weight ratio of 1:4, controlling the slurry concentration to be 10%, carrying out superfine grinding for 35min, and sieving to obtain a white carbon black/titanium dioxide composite material with the average particle size of 1100 meshes; the rest is the same as in preparation example 1.

Example 1

A emamectin benzoate-indoxacarb suspension emulsion is prepared by the following steps:

the vehicle of preparation example 1 and other raw materials were mixed together at the addition amounts shown in table 1, and uniformly dispersed and sheared to obtain a emamectin benzoate-indoxacarb suspoemulsion.

Example 2

the vehicle of preparation example 2 and other raw materials were mixed together at the addition amounts shown in table 1, and uniformly dispersed and sheared to obtain a emamectin benzoate-indoxacarb suspoemulsion.

Example 3

the vehicle of preparation example 3 and other raw materials were mixed together at the addition amounts shown in table 1, and uniformly dispersed and sheared to obtain a emamectin benzoate-indoxacarb suspoemulsion.

Example 4

the vehicle of preparation example 4 and other raw materials were mixed together at the addition amounts shown in table 1, and uniformly dispersed and sheared to obtain a emamectin benzoate-indoxacarb suspoemulsion.

Examples 5 to 13

The Emamectin benzoate-indoxacarb suspoemulsions of examples 5 to 13 were prepared in the same manner as in example 1, except that: the carrier of preparation example 3 was used, and the kinds and the amounts of the respective raw materials were varied, and the details are shown in Table 1.

TABLE 1 compositions and amounts (unit: kg) of Emamectin benzoate-indoxacarb suspoemulsion of examples 1 to 13

Examples 14 to 17

The Emamectin benzoate-indoxacarb suspoemulsions of examples 14 to 17 were prepared in the same manner as in example 1, except that: the carrier of preparation example 3 was used, and bromochlorohydantoin was added to the raw materials, and the types and amounts of the raw materials were varied, as shown in table 2.

TABLE 2 compositions and amounts (unit: kg) of Emamectin benzoate-indoxacarb suspoemulsion of examples 14 to 17

Comparative example 1

The emamectin benzoate indoxacarb suspoemulsion of example 1 of the patent with the publication number CN 101595867B.

Comparative example 2

The emamectin benzoate indoxacarb suspoemulsion of comparative example 2 was prepared in the same manner as in example 3, except that: the surfactant in the raw materials is replaced by equivalent nonylphenol polyoxyethylene ether NP-10, and the types and the mixing amount of the other raw materials are the same.

Comparative example 3

The emamectin benzoate indoxacarb suspoemulsion of comparative example 3 was prepared in the same manner as in example 3, except that: the surfactant in the raw materials is replaced by the same amount of agricultural emulsion No. 600 phenethyl phenol polyoxyethylene ether, and the types and the mixing amount of the other raw materials are the same.

Comparative example 4

The emamectin benzoate indoxacarb suspoemulsion of comparative example 4 was prepared in the same manner as in example 3, except that: the carrier in the raw materials is replaced by bentonite with the same quantity, and the types and the mixing amount of the other raw materials are the same.

Comparative example 5

The emamectin benzoate indoxacarb suspoemulsion of comparative example 5 was prepared in the same manner as in example 3, except that: the carrier in the raw materials is replaced by the precipitated white carbon black which is not subjected to dispersion treatment in an equivalent manner, and the types and the doping amount of the other raw materials are the same.

Comparative example 6

The emamectin benzoate indoxacarb suspoemulsion of comparative example 6 was prepared in the same manner as in example 3, except that: the carrier in the raw materials is replaced by the precipitated white carbon black after dispersion treatment in equal amount, and the types and the mixing amount of the other raw materials are the same.

Comparative example 7

The emamectin benzoate indoxacarb suspoemulsion of comparative example 7 was prepared in the same manner as in example 3, except that: the carriers in the raw materials are replaced by rutile type titanium dioxide which is not dispersed in equal amount, and the types and the mixing amount of the other raw materials are the same.

Comparative example 8

The emamectin benzoate indoxacarb suspoemulsion of comparative example 8 was prepared in the same manner as in example 3, except that: the carriers in the raw materials are replaced by the rutile type titanium dioxide after the dispersion treatment in equal amount, and the types and the mixing amount of the other raw materials are the same.

Performance test 1

The following operations were used to test the performance of the suspending agents of examples 1 to 17 and comparative examples 1 to 8, respectively, and the test results are shown in table 3:

and (3) detecting the granularity: detecting the median diameter D50 of each suspending agent by using a laser particle size distribution instrument;

the overall suspension property is that 1g of the suspending agent is poured into a measuring cylinder filled with 200m L water, stirred for 2min, kept stand for 10min, and the dispersion state of the suspending agent is observed, if the suspended particles are wholly sunk, floated or agglomerated, the suspension property is poor, if the suspended particles are partly sunk, partly floated or partly agglomerated, the suspension property is poor, and if the suspended particles are uniformly dispersed and are not sunk, floated or partly agglomerated, the suspension property is good;

suspension rates of emamectin benzoate and indoxacarb: the detection is carried out by adopting the detection standard and the method of GB/T14825-2006.

TABLE 3 suspending Properties of the suspending agents of examples 1 to 17 and comparative examples 1 to 8

The results in table 3 show that the white carbon black/titanium dioxide composite material prepared by the method is used as a carrier to adsorb the active ingredients of the suspending agent, the median diameter is less than 5 microns, the suspending agent has good suspending performance and is superior to the suspending performance of the emamectin benzoate-indoxacarb suspending agent (comparative example 1) in the prior art, the suspending rate of the emamectin benzoate can reach 99.90 percent at most, the suspending rate of the indoxacarb can reach 99.30 percent at most, and the suspending performance is excellent.

From the results of comparative examples 2 and 3, it was revealed that the suspension performance was lower than that of the present invention, whether aliphatic based polyolefin ethers or aromatic based polyolefin ethers were used; the surfactant in the invention has a great influence on the suspension performance of the suspending agent, probably because the surfactant can enable the surface of the carrier in the suspension system of the invention to form a stable dense adsorption layer, thereby stably adsorbing active ingredients, enabling the active ingredients not to be easily settled or agglomerated and improving the suspension performance of the suspending agent.

As can be seen from comparative examples 4 to 6, the choice of carrier has a great influence on the suspending properties of the suspending agent. The suspending agent obtained by replacing the carrier with bentonite has poor suspending performance; if the precipitated white carbon black is replaced by the precipitated white carbon black which is not subjected to dispersion treatment, the median diameter of particles in the suspending agent is more than 5 mu m, the suspending performance is extremely poor, and the suspending agent is not suitable for spray application. The combination of comparative example 5 and comparative example 6 shows that compared with precipitated silica, rutile type titanium dioxide has a slightly smaller influence on the suspension property of the present invention, probably because the surface hydroxyl of the precipitated silica is more than that of titanium dioxide, and is more prone to multiple agglomeration.

As can be seen from comparative examples 5 and 6, the suspending agent obtained by using the precipitated silica white subjected to the dispersion treatment has better suspension performance than the precipitated silica white which is not subjected to the dispersion treatment. From comparative example 7 and comparative example 8, it can be seen that the suspension using the rutile titanium dioxide after dispersion treatment is superior in suspension performance to the rutile titanium dioxide without dispersion treatment. The synergistic effect of precipitated silica and rutile titanium dioxide is demonstrated by comparative examples 6 and 8 in combination with example 3.

Performance test 2

The following operations were used to test the UV resistance of the suspending agents of examples 1 to 17 and comparative examples 1 to 8, and the results are shown in Table 4:

simultaneously irradiating a sample by 2 parallel 30W ultraviolet lamps, measuring the absorbance of each substance at the corresponding ultraviolet absorption peak by an ultraviolet spectrophotometer and a high performance liquid chromatography, and calculating the residual emamectin benzoate content and the residual indoxacarb content of each substance after different time under ultraviolet irradiation, wherein the distance between the central position of each ultraviolet lamp tube and the liquid level of the solution is 40 cm.

TABLE 4 UV resistance of the suspending agents of examples 1 to 17 and comparative examples 1 to 8 (%)

The detection results in table 4 show that the suspending agent of the present invention has excellent ultraviolet resistance, and the content of the active ingredient in the suspending agent increases first and then tends to be moderate in the same sample within 0-48h of ultraviolet irradiation time, in the ultraviolet resistance of the suspending agent of the present invention, the content of the emamectin benzoate can reach up to 1.58% after 48h of ultraviolet irradiation, the decomposition rate is (2.00-1.58)%/2.00% × 100%: 21%, the content of the indoxacarb can reach up to 14.02%, the decomposition rate is (15.00-14.02)%/15.00% × 100%: 6.53%, the suspending agent in comparative example 1, the content of the emamectin benzoate after 48h of ultraviolet irradiation is 0.11%, the decomposition rate is (0.50-0.11)%/0.50%/× 100%: 78%, the content of the indoxacarb is 0.62%, the decomposition rate is (2.00-0.62)%/2.00)%, 25%: × 100%, and the suspension stability of the suspending agent is better than that of the existing suspending agent.

From comparative examples 2-3, it can be seen that the selection of the surfactant according to the invention has a greater influence on the UV photolytic stability of the suspending agent. From the test results of comparative example 4, it was found that the stability of the suspension concentrate was greatly lowered when the vehicle of the present invention was replaced with a conventional vehicle. The results of comparative examples 6 and 8 in combination with example 3 show that the precipitated silica and rutile type titanium dioxide in the invention have synergistic effect, and the stability of the suspending agent is greatly reduced by singly replacing any dispersed material as a carrier.

The suspending agent can be used as a pesticide and can be suitable for rice leaf rollers, the application mode is spraying, and the application dosage is 10-20 ml/mu.

Test of field drug effect

Summary of the test: the test is carried out in a test field in a farm institute of agricultural sciences in Shandong province, the water and fertilizer conditions of the test field are better, the cultivation and management conditions are consistent, and the soil of the test field is sandy loam.

Control agent 1: the dosage of the 5% emamectin benzoate water dispersible granule of northwest Wigner Biochemical Limited company is 20 g/mu.

Control 2 is a 15% indoxacarb suspension from Dupont, USA, and the usage amount is 8m L/mu.

Blank control, clear water, use amount 15m L/mu.

Test examples 1 to 6 the suspending agents of examples 7, 11 and 14 to 17 of the present invention were used in an amount of 15m L/mu.

Test comparative examples 1-7 the suspending agents of comparative examples 2-8, respectively, were used at 15m L/mu.

Using the apparatus: conventional knapsack sprayer, directional spray.

Water consumption: 30 kilograms of water per mu.

Applying the pesticide 1 time (at peak period of low-age larvae of cnaphalocrocis medinalis) in 15 days of 7 months, repeating for 3 times, and each cell is 100m². After the application, a water layer of 3-5 cm is kept, and the management is normal after 5 days. Adjusted before and after the medicine for 3d, 7d and 14d respectivelyChecking the number of live insects; during investigation, 5-point sampling is adopted, 5-point investigation is carried out at each point, the number of live insects in 25-point investigation is carried out, the control effect is calculated, and specific results are shown in table 5. The calculation formula is as follows:

control effect (%) (1- (number of live insects after drug administration in the drug-treated area of blank area ×)/(number of live insects before drug administration in the drug-treated area of blank area ×)) × 100%.

TABLE 5 results of pharmacodynamic test of cnaphalocrocis medinalis

The test results in Table 5 show that the control effect of the suspending agent on cnaphalocrocis medinalis at 14 days after the suspending agent is applied can reach 97.20 percent at most, and the control effect is superior to that of other medicaments in the market (contrast medicament 1-2). The results of the examples 14 to 17 show that the suspending agent of the invention has a great improvement on the control effect of cnaphalocrocis medinalis by adding a small amount of bromochlorohydantoin. The results of the experimental comparative examples 1 to 7 show that the effect of the carrier on the efficacy of the suspending agent is greater than the effect of the surfactant on the efficacy of the suspending agent. As can be seen from the test comparative example 5 and the test comparative example 7, the precipitated silica and the rutile type titanium dioxide in the carrier have a synergistic effect.

The above-mentioned embodiments are merely illustrative and not restrictive, and those skilled in the art can modify the embodiments without inventive contribution as required after reading this specification, but only fall within the scope of the claims of the present invention.

Claims

1. The emamectin benzoate-indoxacarb suspension emulsion is characterized by being prepared from the following raw materials in percentage by weight: 2-7% of emamectin benzoate, 10-20% of indoxacarb, 3-10% of carrier, 1-3% of surfactant, 5-10% of organic solvent and the balance of water, wherein the carrier is a white carbon black/titanium dioxide composite material.

2. The emamectin benzoate-indoxacarb suspoemulsion of claim 1, which is characterized in that: the average grain diameter of the white carbon black/titanium dioxide composite material is not less than 1000 meshes.

3. The emamectin benzoate-indoxacarb suspoemulsion according to claim 1, wherein the white carbon black/titanium dioxide composite is prepared by the following steps:

4. The emamectin benzoate-indoxacarb suspoemulsion formulation according to claim 3, wherein in step a, the white carbon black is subjected to a dispersion pretreatment as follows: and (3) in the presence of sodium polyacrylate, carrying out superfine grinding on the white carbon black to obtain the white carbon black with the median diameter of 8-12 mu m.

5. The emamectin benzoate-indoxacarb suspoemulsion of claim 3, wherein in step a, the titanium dioxide is subjected to superfine grinding to obtain titanium dioxide with a median diameter of 3-5 μm.

6. The method for preparing the emamectin benzoate-indoxacarb suspoemulsion according to claim 1, characterized in that: the white carbon black is precipitated white carbon black, and the titanium dioxide is rutile titanium dioxide.

7. The emamectin benzoate-indoxacarb suspoemulsion of claim 1, which is characterized in that: the surfactant is one or more of dodecyl trimethyl ammonium bromide, tetradecyl trimethyl ammonium bromide and didecyl dimethyl ammonium bromide.

8. The emamectin benzoate-indoxacarb suspoemulsion of claim 1, which is characterized in that: the organic solvent is one or more of dimethylbenzene, methylbenzene and ethanol.

9. The emamectin benzoate-indoxacarb suspoemulsion as claimed in claim 1, which further comprises the following raw materials in percentage by weight: 0.01 to 0.04 percent of bromine-chlorine hydantoin.

10. A process for the preparation of the emamectin benzoate-indoxacarb suspoemulsion according to any one of claims 1 to 9, which is prepared by the following steps: the raw materials are mixed and dispersed according to the weight percentage, and the emamectin benzoate-indoxacarb suspension emulsion is obtained after shearing.