CN111184021B - Fruit tree seedling root bactericide compounded by tolclofos-methyl and pyraclostrobin and preparation method, use method and application thereof - Google Patents

Abstract

The invention discloses a fruit tree seedling root bactericide compounded by tolclofos-methyl and pyraclostrobin, a preparation method, a use method and an application thereof, wherein the bactericide comprises the following components in percentage by mass: 11.75 percent of effective sterilization component, 0.05 percent of plant growth regulator, 0.5 percent of thickening agent, 8.0 percent of wetting dispersant, 10.0 percent of filler, 0.25 percent of film-forming agent, 0.1 percent of acid-base regulator and 0.5 percent of defoaming agent; the solvent is water; the effective sterilization component consists of tolclofos-methyl and pyraclostrobin in a mass ratio of 10-35: 1; the plant growth regulator is one or more of 6-benzylaminopurine, naphthylacetic acid and 2, 4-dichlorophenoxyacetic acid; the thickener is one or more of sodium carboxymethylcellulose, sodium alginate, bentonite and Arabic resin; the filler is selected from kaolin, white carbon black, light calcium carbonate and diatomite; the film forming agent is selected from xanthan gum, gelatin, sodium silicate and sodium polyacrylate; the defoaming agent is organic silicon. The bactericide has the advantages of simple formula, low cost and wide application range, and has better control effects on southern blight, white stripe disease and other root diseases.

Description

Fruit tree seedling root bactericide compounded by tolclofos-methyl and pyraclostrobin and preparation method, use method and application thereof

Technical Field

The invention relates to a pesticide for preventing and treating diseases of roots of crops, in particular to a bactericide for preventing and treating diseases of roots of fruit tree seedlings, and a preparation method, a use method and application thereof.

Background

Fruit trees are important economic crops, the planting area is wide, the economic value of products is high, but the yield and the quality of fruits are easily reduced due to root diseases in the fruit tree planting process, and great loss is brought to fruit growers.

The root diseases are important diseases of fruit trees and have great influence on the growth and fruit bearing of the fruit trees. When the roots of newly planted young trees are infected by pathogenic bacteria, rotten roots, root stem necrosis, root cancer and the like can be caused, and the growth and development of the light trees are poor, and the heavy trees are dead. The newly planted fruit tree seedling is easy to be infected by pathogenic bacteria due to the reasons of more root wounds, poor disease resistance and the like. After the root is infected, the root can carry bacteria for a lifetime, and the influence on the growth of the tree body is large. Among the common diseases of the root of the fruit tree, there are southern blight, white streak feather disease, root rot disease, purple streak disease, round spot root rot, root canceration, hairy root and the like. At present, the fungal diseases which are relatively common and have relatively serious harm on fruit tree seedlings mainly comprise southern blight and white streak disease.

Southern blight, also known as sclerotic root rot and sclerotic seedling blight, is a commonly occurring plant disease in tropical and subtropical regions, and the pathogen of southern sclerotium rolfsiusacc. The sclerotium rolfsii has a wide host range and can harm various plants. On fruit trees, southern blight mainly infects the neck of the root of a young tree, so that dead trees are caused, and seedlings and the young tree are seriously damaged. Sclerotium of sclerotium grows and extends to reach the root neck of tree body in hot and rainy season, and surrounds the root neck, resulting in root neck broken layer and rot.

Leaf scald disease is caused by an infection with hypocrea fusca (Roselliannecatax). The Mucuna alba can survive in soil for a long time. The roots of the newly-planted seedlings are infected by the contact of germs, the capillary roots of the germs invade, the growth extends to the main roots, the root rot is caused, the tree vigor is weak, the growth is retarded, the leaves turn yellow, the early fall off is caused, and finally the whole tree dies.

At present, no effective control method and no effective control agent exist for the fruit tree root diseases. When symptoms appear on the overground part of the fruit tree, the symptoms are often in the late stage of disease attack, and the disease cannot be rescued; as a remedy, the diseased root is dug out, cut off, aired, sterilized by soil and then backfilled; as an early preventive measure, a high-concentration bactericide can be prepared by using a conventional organic bactericide such as carbendazim, and roots are irrigated in spring. Because the measure has large dosage and poor prevention effect, the measure is rarely used in actual production.

Therefore, the prior art has yet to be developed.

Disclosure of Invention

Aiming at the current situation that effective prevention and control agents for fruit tree root diseases are lacked in actual production, the applicant develops and provides a fruit tree seedling root bactericide for effectively preventing the fruit tree root diseases, a preparation method and a use method thereof, so that the bactericide is used for treating roots of fruit tree seedlings before field planting, pathogenic bacteria are prevented from infecting from root wounds at the initial stage of seedling field planting, and the incidence rate of newly planted young trees is greatly reduced.

The technical scheme of the invention is as follows:

1. the invention provides a fruit tree seedling root bactericide for preventing and treating root diseases, which is prepared by compounding tolclofos-methyl and pyraclostrobin, and comprises an effective bactericidal component, a plant growth regulator and an auxiliary agent, wherein the effective bactericidal component consists of the tolclofos-methyl and the pyraclostrobin in a mass ratio of 10: 1-35: 1; wherein the plant growth regulator is one or more of 6-benzylaminopurine, naphthylacetic acid and 2, 4-dichlorophenoxyacetic acid.

Tolclofos-methyl, also called as rickets and tolclofos, is a broad-spectrum systemic fungicide specially used for preventing and treating soil-borne diseases, mainly plays a role in protection, has strong adsorption effect, is not easy to run off, has long lasting period and has certain lasting period in soil. Has good control effect on diseases caused by fungi of semi-known fungi, basidiomycetes and ascomycetes, and can be used for controlling diseases caused by rhizoctonia solani, sclerotinia rolfsii, phanerochaete and sclerotinia on cotton, potatoes, beet, fruit trees and ornamental plants. Has good control effects on rhizoctonia rot, fusarium wilt, sclerotinia rot, root rot, cruciferous black root, brown rot and the like, and also has good control effects on seedling blight bacteria with resistance to quintozene.

Pyraclostrobin (pyraclostatin) is a broad-spectrum fungicide, an inhibitor of mitochondrial respiration, and mitochondria are unable to produce and supply energy for cellular metabolism, ultimately leading to cell death. Pyraclostrobin has good control effect on diseases caused by fungi of ascomycetes, basidiomycetes, deuteromycetes and oomycetes. Has good inhibition effect on spore germination and hypha growth, can be used as protective and therapeutic bactericide, and has long lasting period and rain wash resistance.

In the invention, the effective sterilization components are as follows: the mass ratio of tolclofos-methyl to pyraclostrobin is 10: 1-35: 1; preferably, the mass ratio of the tolclofos-methyl to the pyraclostrobin is 45:2, namely the content of the tolclofos-methyl raw powder in the preparation is 11.25%, the content of the pyraclostrobin raw drug is 0.5%, under the content condition, the synergistic effect between the two components is strongest, and the sterilization effect is best.

The plant growth regulator is selected from one or more of 6-benzylaminopurine, naphthylacetic acid and 2, 4-dichlorophenoxyacetic acid, and the mass percentage concentration of the plant growth regulator is 0.01-0.5%; preferably, the mass percentage concentration of the 6-benzylaminopurine is 0.05%, and the purity of the 6-benzylaminopurine raw material is not lower than 98%.

The wetting dispersant is selected from one or more of SP-SC29, SP-2728, DS-1287, 92FS1 and 33SC, and the mass percentage concentration of the wetting dispersant is 6-12%; the optimal wetting dispersant is a compound mixture formed by mixing liquid SP-2728 and liquid SP-SC29 according to a ratio of 5:3, and the mass percentage concentration of the liquid SP-2728 and the liquid SP-SC29 in the bactericide is 5.0% and 3.0% respectively.

The thickening agent is selected from one or more of sodium carboxymethylcellulose, sodium alginate, bentonite and arabic resin, and the mass percentage concentration of the thickening agent is 0.25-1.0%; the best thickener is sodium carboxymethyl cellulose, and the content is 0.5%; the purity of the sodium carboxymethylcellulose raw material is not less than 98%.

The filler is selected from one or more of kaolin, white carbon black, light calcium carbonate and diatomite, and the mass percentage concentration of the filler is 7.0-13.0%; the most preferred filler is kaolin, which is present in an amount of 10.0%.

The film forming agent is selected from one or more of xanthan gum, gelatin, sodium silicate and sodium polyacrylate, and the mass percentage concentration of the film forming agent is 0.15-0.5%; the optimal film forming agent is sodium silicate, and the content is 0.25%; the modulus of sodium silicate is 3.3.

The defoaming agent is organic silicon, and the mass percentage concentration of the organic silicon is 0.25-1%, and the preferable concentration is 0.5%.

Acid-base regulator: citric acid is selected, and the mass percentage concentration of the citric acid is 0.05-0.2%. The preferred content thereof is 0.1%.

The solvent is water, preferably secondary water or more.

In a preferred embodiment, the bactericide for the roots of the fruit tree seedlings comprises the following components in percentage by mass: 3.9-35% of effective bactericidal component, 0.01-0.5% of plant growth regulator, 0.25-1.0% of thickening agent, 6.0-12.0% of wetting dispersant, 7.0-13.0% of filler, 0.15-0.5% of film-forming agent, 0.05-0.2% of acid-base regulator and 0.25-1% of defoaming agent; the solvent is water.

Further, in order to prolong the lasting period of the bactericide, the following components can be added to the basic formula of the bactericide for the root of the fruit tree seedling:

an antifreezing agent: one or more of ethanol, glycerol, urea and sodium chloride can be selected, and the mass percentage concentration of the one or more of ethanol, glycerol, urea and sodium chloride is 2.5-7.5%; most preferably 5.0% (purity ≧ 99%), and the cold storage property of the preparation after addition is best.

Preservative: selecting 1, 2-benzisothiazolin-3-one with the mass percentage concentration of 0.025-0.1%; the preferred concentration is 0.05% and the purity of the 1, 2-benzisothiazolin-3-one starting material is not less than 98%.

Warning color: selecting neutral black with the mass percentage concentration of 0.025-0.1%, and the optimal concentration of 0.05%;

nutrient substances: sucrose, glucose, maltose and the like are selected, and the mass percentage concentration of the sucrose, the glucose, the maltose and the like is 0.5-2%, and the optimal concentration is 1.0%. The nutrient can promote absorption of effective components and growth active substances.

In the most preferred embodiment, the formula of the bactericide for the roots of the fruit tree seedlings is as follows: 11.25% of tolclofos-methyl, 0.5% of pyraclostrobin, 8.0% of compound wetting dispersant, 0.5% of sodium carboxymethylcellulose, 10.0% of kaolin, 0.25% of sodium silicate, 5.0% of urea, 0.05% of neutral black, 0.1% of citric acid, 0.05% of 6-BA, 0.05% of 1, 2-benzisothiazolin-3-one, 0.5% of organic silicon, 1.0% of cane sugar and the balance of water; wherein the compound wetting dispersant is a mixture of SP-2728 and SP-SC29 with the mass ratio of 5: 3. The formula has the best prevention and treatment effect on the root germs of the fruit tree seedlings, and has the best comprehensive performances such as film forming performance, lasting period and the like, and the lasting period is prolonged to 30-60 days.

2. The invention also provides a preparation method of the fruit tree seedling root bactericide, which comprises the following steps:

1) uniformly mixing the effective bactericidal component, the filler, the wetting dispersant, the plant growth regulator, the thickening agent and the film forming agent, adding 40-50% of the total water, performing primary sanding, and treating for 30-60 min;

2) then adding warning color, antifreezing agent and 20-30% of the total water amount, and performing secondary sanding for 30 min;

3) finally, adding a defoaming agent, an acid-base regulator, a preservative, nutrient substances and the rest water, and performing sanding for the third time for 60 min;

4) separating the sand from the sand medium, shearing and emulsifying for 10min with a shearing machine to obtain a preparation; and (5) after the quality inspection is qualified, obtaining the bactericide for the roots of the fruit tree seedlings, and packaging the bactericide into a finished product.

3. The invention also provides a quality inspection method of the fruit tree seedling root bactericide, which comprises the following steps:

the quality inspection indexes mainly comprise suspension rate, viscosity, pH value, centrifugal stability, pourability, particle size, dispersibility in water, low-temperature stability, heat storage stability and the like, and each quality inspection index and a corresponding quality inspection method are as follows:

suspension percentage: the suspension rate of the finished preparation is qualified when the suspension rate is not less than 90 percent by referring to the GB/T14825-2006 pesticide suspension rate determination method;

viscosity: putting 200mL of the processed preparation into a beaker, and standing in a constant-temperature water bath at 25 ℃ for 1 hour; adjusting the viscometer to be normal, adjusting the rotation speed of a rotor to (30 +/-1) rpm, slowly inserting the rotor into the sample to enable the liquid level to just submerge a groove on the rotor, starting an engine, and immediately reading the viscosity value (mPa & s) after 1 min; the viscosity of the finished product preparation is qualified when the viscosity is required to be 200-400 mPa.s;

pH value: weighing 1g of the processed preparation in a 100mL beaker, adding distilled water which is boiled newly and cooled to room temperature, stirring vigorously for 1 minute, standing for 1 minute, measuring the pH value by using a pH meter, repeating for 3 times, and calculating the average value; the pH of the finished product preparation is required to be between 6.0 and 7.5 to be qualified;

centrifugal stability: adding 5mL of the processed preparation into a 5mL conical glass tube with scales, centrifuging at 3000rpm for 30min, taking out, and observing and recording the conditions of water precipitation and precipitation; the water precipitation amount of the finished product preparation after centrifugation is less than 3 percent of the volume requirement of the processed preparation, and the finished product preparation is qualified;

pourability: weighing 100mL measuring cylinder after drying, loading the processed preparation into the measuring cylinder with the volume of 8/10 of the measuring cylinder, weighing, sealing, and standing for 24 hours. Rotating the measuring cylinder by an angle of 135 degrees, and pouring for 1 minute; inverting for another 1 minute, and weighing the residue after pouring; then, weighing the measuring cylinder and the mass of the residue, and calculating the residual amount of the wall hanging; the pouring residue of the finished preparation is required to be lower than 3.0 percent, and the wall built-up residue is lower than 1.0 percent, so that the finished preparation is qualified;

particle size: detecting the diameter of the preparation particles in the preparation by using a laser particle size detector; the grain size index D50 of the finished product preparation is required to be less than 5.0 microns and is a qualified standard;

dispersibility in water: taking a 100mL measuring cylinder, filling 99.5mL standard hard water, taking 0.5mL sample by using an injector, dripping the sample into water from a position 5cm away from the water surface of the measuring cylinder, and observing the dispersion state of the sample; the finished product preparation is required to be automatically dispersed in water in a cloud state, and no visible particles or flocculent sinking is qualified;

low-temperature stability: placing 80mL of sample in a 100mL beaker, keeping the temperature at (0 +/-1) DEG C for l hours, stirring the sample once every 15min for 15 seconds every time, and observing the appearance change of the sample; then sealing, continuously standing for 7 days at (0 +/-1) DEG C, taking out, recovering to room temperature, and carrying out several index tests such as suspension rate, viscosity, pH value and the like; after the finished product preparation is placed for 7 days at low temperature, the suspension rate, the viscosity and the change amplitude of the pH value are required to be not more than 1 percent, and the finished product preparation is a qualified product;

heat storage stability: detecting the content of effective bactericidal components in the preparation, injecting 30mL of sample into 3-5 clean ampoules by using an injector, sealing by using high-temperature flame, and weighing respectively; and (3) placing the sealed ampoule bottle in a thermostat at 54 +/-2 ℃, taking out after placing for 14 days, detecting indexes such as suspension rate, viscosity, pH value and the like, and simultaneously detecting the content of effective components in the heat storage preparation. After the finished product preparation is stored thermally, the requirement of the relative digestion rate of the effective sterilization components is lower than 5.0 percent, the requirement of the suspension rate is more than or equal to 85 percent, and the requirement of the variation amplitude of other indexes after thermal storage is less than 1 percent, thus the finished product is qualified.

Film forming time: uniformly coating the sample on a glass slide by using a brush pen, placing the glass slide in a thermostat at 25 ℃ for airing, and recording the time required for completely drying the glass slide; the film forming time of the finished product preparation is required to be less than 30 minutes and is qualified;

film forming effect: after the glass slide is dried, observing the film forming condition and appearance of the surface of the glass slide; the finished product preparation is required to be capable of forming a film on the surface of the glass slide uniformly, the film layer is not cracked, and the surface is flat and qualified;

water resistance: uniformly smearing the sample on the glass slide by using a brush pen, immersing the glass slide into water after the glass slide is dried, soaking for 12 hours, and observing the falling condition of the sample in the water; the film layer of the finished product preparation is required to be complete, and the falling area is not more than 20 percent and is qualified;

adhesion force: uniformly coating a sample on a glass slide by using a brush pen, immersing the glass slide in a beaker filled with 250mL of water after the glass slide is dried, placing the beaker in an ultrasonic cleaning instrument, oscillating for 5 minutes, and observing the falling condition of a film layer; the product preparation is qualified when the falling area requirement is less than 20%;

after all the indexes are qualified, the bactericide can be ensured to have more stable performance, the medicament can be firmly attached to the root of a seedling to form a uniform protective film, and active ingredients are uniformly dispersed into the film, so that the effect of the active ingredients is exerted to the maximum extent.

4. The invention also provides a use method of the fruit tree seedling root bactericide

When treating the nursery stock, diluting the bactericide for the root of the nursery stock into liquid medicine of 25-150 times, soaking the root of the nursery stock of the fruit tree in the liquid medicine for 10-30min, and planting the nursery stock with the liquid medicine;

when the seeds are treated, the bactericide and the seeds are mixed according to the mass ratio of 1:25-50, a small amount of water is added to prepare a medicament, the medicament is uniformly attached to the surfaces of the seeds, and the seeds are aired for sowing.

Advantageous effects

Different from the existing bactericide, the bactericide for the roots of the fruit tree seedlings provided by the embodiment of the invention has the following beneficial effects:

1) a protective film layer can be formed on the root of the seedling, the film layer can be permeable to water and air, can promote the growth of the root or does not influence the growth of the root, and can prevent pathogenic bacteria from infecting the root;

2) the film layer can bear soaking and scouring of irrigation water and does not fall off or disappear in a longer time;

3) has the advantages of slow release and long duration: the film layer contains broad-spectrum bactericidal components with systemic protection, the bactericidal components are gradually released from the film after use, the growth and the expansion of germs to roots are inhibited, and the bactericidal components can be kept for a long time in the film layer;

4) has no harm to the root of the crop, belongs to an environment-friendly preparation and is convenient to use.

5) The fruit tree seedling root bactericide has a simple formula and low production cost; the production and processing are simple and convenient, and the large-scale production is convenient; the bactericide has wide application range and better prevention effect on southern blight, white stripe disease and other root diseases.

Detailed Description

The present invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the description of the embodiments is only for illustrating the present invention and should not be taken as limiting the invention as detailed in the claims. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

Materials and methods

1 test Material

95% of tolclofos-methyl raw powder (from hong Kong Dong gold chemical Co., Ltd.); 99.3 pyraclostrobin original drug (available from technologies ltd. of Qingdao); a 25% pyraclostrobin suspension (Shandong Kangqiao biology, Inc.); 25g/L pyraclostrobin suspension seed coating (Zymond Switzerland).

Wetting and dispersing agent: SP-SC29 (Jiangsu Optimus chemical industry); SP-2728 (Jiangsu Optimus chemical industry); 92FS1 (shanghai star chemical engineering); 33SC (starfish flying chemical); DS1287 (Beijing Guangyuan Yinong).

Film-forming agent: xanthan gum (tianjin optometry chemical research institute); gelatin (Tianjin Guangcheng Chemicals, Inc.);

sodium polyacrylate; sodium silicate (Shandong Youso chemical).

Thickening agent: sodium carboxymethylcellulose (national pharmaceutical group chemical reagents limited); bentonite; an arabic resin; sodium alginate (Zhejiang Green source food Biotech Co., Ltd.).

An antifreezing agent: ethanol (Tianjin Funing Fine chemical Co., Ltd.); glycerol (Tianjin north coupled fine chemicals development, ltd); urea (laiyang condrd chemical); sodium chloride (Laiyang Kande chemical).

Filling: light calcium carbonate; diatomaceous earth (Tianjin Kaitan chemical reagent); white carbon black; kaolin (Shanghai Zhanyun chemical industry).

Warning color: neutral black (parentage of Hubei).

Defoaming agent: organosilicon (Shandong Youso chemical industry).

Preservative: 1, 2-benzisothiazolin-3-one (BIT, a leaf organism from Shanghai).

Acid-base regulator: sodium citrate (Tianjin Guangfu chemical research institute).

Organic nutrient: sucrose (Tianjin North Union Fine chemical development Co., Ltd.).

2. Quality detection method of root bactericide

(1) And (3) suspension rate determination: a, B aliquots of 5.0g each (to the nearest 0.02g, less than 0.1g) were weighed into 200mL beakers, 50mL of standard hard water (30. + -.1 ℃) was added, shaken by hand for 1-2min in a circular motion at 120r/min, transferred to 250mL graduated cylinders and diluted to the mark using standard hard water (30. + -. 1 ℃) and the cylinders were inverted approximately 30 times within 1min centered on the cylinder bottom with a stopple. The 9/10 (i.e., 225mL) solution in the volume of the sample A cylinder was immediately removed with a pipette at around 10s to ensure that the tip of the pipette was always 5mm below the liquid level. The remaining 25mL of solution was transferred to a beaker with a volume of 100mL which had been dried to constant weight, transferred to a drying oven at a temperature of 80-90 ℃ to dry to approximately 2mL, 1mL of ethanol was added, drying was continued in the oven to constant weight and weighed (to an accuracy of 0.02g) to give a residue with a mass ma. And (3) vertically putting the group B into a constant-temperature water bath (30 +/-1 ℃), sucking 9/10 volumes of solution from the group A by using a suction pipe after 0.5h, drying according to the method A, and weighing to obtain the residue mass mb. The suspension ratio X (%) of the sample was calculated by the following formula:

in the formula: ma is the dried mass g of the residual 25mL of the suspension liquid in the measuring cylinder A;

mb is the dried mass g of the remaining 25mL of the suspension liquid in the measuring cylinder B;

(2) and (3) pH value measurement: weighing 1.0g (accurate to 0.02g, with the difference less than 0.1g) of the root bactericide sample, placing the root bactericide sample in a 100mL beaker, adding 100mL of newly prepared distilled water, stirring with a glass rod for 1min, standing for 1min, inserting the debugged and washed saturated calomel electrode into the glass electrode sample solution, and measuring the pH value. The measurement was repeated 3 times, and the arithmetic mean value thereof was used as the pH value of the group of samples.

(3) Measurement of viscosity: and (3) fully and uniformly shaking the sample, putting 200mL of sample to be detected in a beaker, and standing for 1h at the temperature of 25 ℃. Then with the viscometer debugging normal, then select corresponding rotor, slowly insert the sample with the rotor in, make the recess on the rotor just by liquid level submergence. Starting the engine, gradually adjusting to the highest speed, then reducing to the proper and same rotating speed (about 30 +/-1 r/min), and reading the dial number after 1 min.

η＝k×α

Eta- -viscosity of the sample, in mPas;

k- -coefficient of rotor in rotational viscometer coefficient table;

alpha-reading in the rotational viscometer scale.

(4) And (3) determining the water-entering dispersibility: adding 99.5mL of standard hard water into a 100mL measuring cylinder, sucking 0.5mL of root bactericide sample to be measured by using a pipette, slowly dripping the bactericide sample into the standard hard water from a position 5cm away from the horizontal plane of the measuring cylinder, immediately observing the dispersion condition of the sample in the water, and classifying the sample into a good grade, a good grade and a poor grade according to the dispersion state.

And (3) excellent: the water automatically disperses in fog form after entering water, and no visible block sinks.

Good: the dispersion is self-dispersing after water entry, with a small amount of particles sinking, but a small amount of lumps sinking may be slowly dispersed or dispersed after slight shaking.

Difference: the water can not be automatically dispersed after entering water, a large amount of blocks sink, and the water can be dispersed or can not be dispersed after being strongly and violently shaken.

(5) And (3) centrifugal stability determination: adding 4mL of sample to be detected into a 4mL centrifuge tube (with scales), centrifuging at the speed of 3000rpm for 20-30min, taking out, observing the volume of separated water and sediment, and dividing the volume of separated water and sediment into three stages, namely a superior stage, a good stage and a poor stage.

And (3) excellent: the water separating volume and the precipitation volume are less than 2 percent or no water separating precipitation exists;

good: the water separating volume and the precipitation volume account for 2 to 5 percent;

difference: the water separating volume and the precipitation volume are more than 5 percent.

(6) And (3) detecting the pourability: taking a proper amount of sample, quickly placing the sample in a weighed measuring cylinder (including a plug) until the volume of the measuring cylinder is about 8/10 points, plugging the plug, weighing, and placing for a certain time (12h-24 h). And (3) opening the plug, rotating the measuring cylinder by 135 degrees to ensure that the measuring cylinder is poured for about 1min, vertically inverting for 1min, and weighing the measuring cylinder and the plug again. Adding water with the volume equivalent to 80% of that of the measuring cylinder into the measuring cylinder, plugging the plug tightly, turning the measuring cylinder upside down for more than ten times, pouring the water in the measuring cylinder again according to the operation, and then weighing the mass of the measuring cylinder and the plug again.

X1＝[(m2-m0)]/[(m1-m0)]×100

X2＝[(m3-m0)]/[(m1-m0)]×100

In the formula: m 0-cylinder, plug constant mass, g;

m 1-mass of cylinder, stopper and sample, g;

m 2-mass of cylinder, stopper and remaining sample after pouring, g;

m 3-mass of cylinder, stopper and remaining sample, g, after washing.

And (3) excellent: the residual sample/%, after pouring, is less than or equal to 3.0, and the residual sample/%, after washing, is less than or equal to 1.5;

good: the remaining sample after pouring/% ≦ 6.0 and >3.0, the remaining sample after washing/% ≦ 3.0 and > 1.5;

difference: the sample/% > 6.0 remained after pouring and the sample/% >3.0 remained after washing.

(7) And (3) detection of particle size: the diameter of the formulation particles in the formulation was checked using a laser particle size detector. General suspending agent D₅₀The product is qualified when the particle size is 0.1-5.0 nm.

(8) Film formation time and film formation effect: the sample was evenly spread on the slide with a brush pen, placed in a 25 ℃ incubator and dried, and the time required for complete drying was recorded. After being dried, the appearance and the film forming condition of the film on the surface of the glass slide are observed, and the three-level standards of excellent pourability, good pourability and poor pourability are as follows:

and (3) excellent: uniformly forming a film;

good: the film can be formed, and the surface of the film is slightly uneven;

difference: the film could not be formed uniformly, the film was broken into pieces, and the film was extremely uneven.

(9) And (3) water resistance measurement: evenly paint the sample on the glass slide by using a writing brush, immersing the glass slide into water after the glass slide is dried, soaking for 12 hours, observing the falling condition of the sample in the water, and dividing the sample into three grades of good quality and poor quality:

and (3) excellent: the sample on the slide is relatively complete, and the shedding area does not exceed 1/3;

good: the sample on the slide was retained with a drop area exceeding 1/3 but below 2/3;

difference: the sample on the slide mostly fell off, and the area of the fell off exceeded 2/3.

(10) And (3) measuring the adhesion force: uniformly coating a sample on a glass sheet by using a writing brush, immersing the glass sheet in a beaker filled with 250mL of water after the glass sheet is dried, placing the beaker in an ultrasonic cleaning instrument, vibrating for 5min, observing the falling condition of the beaker, and classifying the beaker into two grades of qualified and unqualified:

and (4) qualification: the sample retention area on the slide is greater than or equal to 1/3;

unqualified: the sample retention area on the slide was less than 1/3.

(11) Appearance and flowability measurement: generally a liquid that flows uniformly, should not cake, can precipitate or delaminate slightly on long term storage, but can recover rapidly on hand shaking at room temperature, and its color.

(12) Determination of Heat storage stability: 30mL of sample is sucked by a syringe, added into a clean reagent bottle and sealed by a paraffin sealing film to prevent sample loss. At least 3 bottles were sealed and weighed separately. And (3) placing the sealed reagent bottle in a thermostat with the temperature of 54 +/-4 ℃, taking out after placing for two weeks, weighing the mass of the reagent bottle, taking a sample with unchanged mass, and inspecting the particle size and the suspension rate within 24 h. After heat storage, the suspension rate, particle size, pH value and the like are all in standard ranges.

(13) Determination of the Low temperature stability: 80mL of the sample was placed in a beaker having a volume of 100mL, and the beaker was left at (0. + -. 2) ℃ for 1 hour, and stirred with a glass rod every 15 minutes for 15 seconds to observe whether the appearance of the sample was changed. And sealing the beaker, placing the beaker at the temperature of (0 +/-2) DEG C for a week, taking out the beaker after a week, firstly returning the beaker to the room temperature, and then detecting the properties of the beaker, such as particle size, viscosity and the like. And comparing the detection results, wherein the detection result is qualified within the standard range.

The above test methods are the test methods for the basic properties employed in the primary formulations of each example 3 in this embodiment.

Example 1: pyraclostrobin and tolclofos-methyl composition proportioning experiment

In this experiment, southern blight (obtained from Yiyuan of Shandong, the same below) was used as a test strain. Culturing the separated and purified strain in potato agar (PDA) culture medium at 25 deg.C for 3 days, and beating with 0.5cm perforator to obtain bacterial cake when the colony radius reaches 2/3.

The inhibition effect of pyraclostrobin and tolclofos-methyl on mycelial growth of sclerotium rolfsii is determined by a mycelial growth rate method. Pyraclostrobin and tolclofos-methyl are respectively prepared into liquid medicines of 0.1 mu g/mL (ppm) and 1.5 mu g/mL (ppm), and are mixed according to the volume ratio of 0:10, 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 3:7, 2:8, 9:1 and 10:0, and the mixture is treated by 11 medicaments, and water is used as a blank control. Mixing the liquid medicine with PDA culture medium, inoculating sclerotium cake of southern blight bacteria to the center of PDA plate, and culturing at 25 deg.C. When the growth diameter of the control hypha reaches 2/3, measuring the colony diameter by a cross method, and calculating the inhibition rate, the toxicity ratio (the ratio of the actual inhibition rate to the expected inhibition rate) and the corrected toxicity ratio (the toxicity ratio/the single-dose average toxicity ratio) of the medicaments with different proportions on the hypha growth of the sclerotium rolfsii; all experiments were repeated three times.

Evaluation criteria: when the corrected toxicity ratio is greater than 1.5, the two agents are considered to have synergistic effects; when the corrected virulence ratio is less than 1.0, both agents are considered to be antagonistic; when the corrected toxicity ratio is 1.0-1.5, the two agents are considered to have additive effects.

The test results are shown in Table 1. When the mass ratio of the pyraclostrobin to the tolclofos-methyl is 1:60-1:135, the pyraclostrobin and the tolclofos-methyl have obvious antagonistic action; when the mass ratio of the two medicaments is between 1:6.429 and 1:35, the treatment synergistic effect is obvious, and particularly when the ratio is 1:22.5, the correction toxicity ratio is the maximum treatment in a test group, and the synergistic effect is strongest.

TABLE 1 inhibitory effect of tolclofos-methyl and pyraclostrobin in different ratios on mycelial growth of sclerotium rolfsii

Example 2: toxicity determination of pyraclostrobin and tolclofos-methyl ratio combination

When the mass ratio of the pyraclostrobin to the tolclofos-methyl is 1:22.5, the inhibition effect of the pyraclostrobin on the hypha growth of sclerotium rolfsii and leptospirillum cellaraense (collected from a tobacco station) is measured by a hypha growth rate method. The concentrations of the drugs were 11.7, 5.9, 2.9, 1.5, 0.7, 0.4, and 0.2. mu.g/mL (ppm), respectively, and the drug solutions were mixed with PDA, and the solvent was used as a blank control. Inoculating the fungus cakes of sclerotium rolfsii and leptospirillum albopictus to the center of a PDA (personal digital Assistant) flat plate containing a medicament, culturing at 25 ℃, measuring the diameter of a colony by a cross method when the growth diameter of hyphae subjected to control treatment reaches 2/3 of the diameter of a culture dish, calculating the inhibition rate of the medicament on the growth of the hyphae of the medicament, fitting a toxicity regression equation, and calculating EC50, correlation coefficients and compound co-toxicity coefficients.

Mixed single theory virulence index (TTI) ═ sigma (single virulence index TI multiplied by the ratio P of single virulence)

The test results are shown in Table 2. When the mass ratio of the pyraclostrobin to the tolclofos-methyl is 1:22.5, the cotoxicity coefficient of the mixed preparation for the treatment of the two pathogenic bacteria is far greater than 120; when the two medicines are mixed, the EC50 for sclerotium rolfsii and sclerotinia sclerotiorum is 0.55 μ g/mL and 2.78 μ g/mL respectively.

TABLE 2 toxicity of tolclofos-methyl and pyraclostrobin (1:22.5) against southern blight and hairy vein blight

Example 3

According to the formula of the following table 3, 9 experimental groups of primary preparations were prepared, and the suspension rate, viscosity, pourability, centrifugal stability film forming effect, and dispersibility in water of the primary preparations of each experimental group were measured, and the comprehensive properties of the primary preparations of each experimental group were compared, and the test results are specifically shown in table 4.

TABLE 3 experimental group setup protocol

Table 4 test results of different experimental groups

The results show that the comprehensive performance of the 9 experimental groups is good, wherein the comprehensive performance of the experimental group 8 is optimal, the suspension rate is highest, the viscosity is moderate, the film forming time is short, and the film forming effect is excellent.

Example 4: processing and quality detection of root bactericide

1. The embodiment provides a bactericide for the root of a fruit tree seedling, which consists of the following components: 11.25% of tolclofos-methyl, 0.5% of pyraclostrobin, 8.0% of compound wetting dispersant, 0.5% of sodium carboxymethylcellulose, 10.0% of kaolin, 0.25% of sodium silicate, 5.0% of urea, 0.05% of neutral black, 0.1% of citric acid, 0.05% of 6-BA, 0.05% of 1, 2-benzisothiazolin-3-one, 0.5% of organic silicon, 1.0% of cane sugar and the balance of water; wherein the compound wetting dispersant is a mixture of SP-2728 and SP-SC29 with the mass ratio of 5: 3.

2. The preparation method of the root bactericide comprises the following steps:

A. uniformly mixing a tolclofos-methyl technical product, a pyraclostrobin technical product, kaolin, SP-2728+ SP-SC29, 6-benzylaminopurine, sodium carboxymethylcellulose, sodium silicate and 150mL of water, sanding for 60min, grinding effective ingredients into particles with the diameter of less than 5 micrometers, and fully mixing the particles with a filler and a wetting dispersant;

B. adding neutral black, urea and 100mL of water, and sanding for 30min to prepare slurry;

C. finally, adding organic silicon, citric acid, 1, 2-benzisothiazolin-3-one, sucrose and the rest water, adjusting the pH value by using an acid-base regulator, sanding for 60min, and fully grinding and mixing all the raw materials to improve the physical and chemical properties of the medicament;

D. and (4) separating the sand grinding object from the sand grinding medium, and shearing and emulsifying for 10min by using a shearing machine to prepare the bactericide for the root of the fruit tree seedling.

The bactericide for the root of the fruit tree seedling is subjected to detection of various indexes, and the detection result is shown in the following table 5.

Example 5: processing and quality detection of root bactericide

The embodiment provides a bactericide for the root of a fruit tree seedling, which consists of the following components: 5.625 percent of tolclofos-methyl, 0.25 percent of pyraclostrobin, 6.0 percent of compound wetting dispersant, 0.25 percent of sodium carboxymethylcellulose, 7 percent of kaolin, 0.15 percent of sodium silicate, 2.5 percent of urea, 0.025 percent of neutral black, 0.05 percent of citric acid, 0.025 percent of 6-BA, 0.025 percent of 1, 2-benzisothiazolin-3-one, 0.25 percent of organosilicon, 0.5 percent of sucrose and the balance of water; wherein the compound wetting dispersant is a mixture of SP-2728 and SP-SC29 with the mass ratio of 5: 3.

The treating agent of this example was prepared in the same manner as in example 4. The bactericide for the root of the fruit tree seedling is subjected to detection of various indexes, and the detection result is shown in the following table 5.

Example 6: processing and quality detection of root bactericide

The embodiment provides a bactericide for the root of a fruit tree seedling, which consists of the following components: 22.5% of tolclofos-methyl, 1.0% of pyraclostrobin, 12.0% of compound wetting dispersant, 1% of sodium carboxymethylcellulose, 13.0% of kaolin, 0.5% of sodium silicate, 7.5% of urea, 0.1% of neutral black, 0.2% of citric acid, 0.1% of 6-BA, 0.1% of 1, 2-benzisothiazolin-3-one, 1.0% of organic silicon, 2.0% of sucrose and the balance of water; wherein the compound wetting dispersant is a mixture of SP-2728 and SP-SC29 with the mass ratio of 5: 3.

The treating agent of this example was prepared in the same manner as in example 4. The bactericide for the root of the fruit tree seedling is subjected to detection of various indexes, and the detection result is shown in the following table 5.

TABLE 5 detection results of bactericide for root of fruit tree seedling

From the data in table 5, it can be seen that: the root fungicides provided in examples 4 to 6 all meet the detection standards in terms of various detection indexes, and particularly, the root fungicide provided in example 4 has the best overall performance and is excellent in adhesiveness, heat storage property and pourability.

Comparative example 7

1 experimental group and 5 control groups were set. Root fungicides were prepared using the formulation of example 4 for each group, but the addition procedure was different for each group.

In each group, the effective bactericidal component, the plant growth regulator and the wetting dispersant are added as the first part; then, the filler, the thickener and the film forming agent were used as group a, the antifreeze and the warning color were used as group B, the defoamer, the preservative, the nutrient substance and the like were used as group C, the three groups were combined and arranged, and after the grinding treatment was performed according to the method of example 4, the pH adjuster was added to adjust the pH value, and finally the preparation was obtained, and the quality of each group of preparations was checked. The addition sequence of the auxiliary agents in the 6 groups is shown in the following table 6, and the quality detection results of the 6 groups of preparations are shown in the table 7.

TABLE 6 auxiliary addition sequence table for experimental and control groups

Group of	Firstly, use	In	Rear end
				Experimental group	A	B	C
Control group 1	A	C	B
				Control group 2	B	A	C
Control group 3	B	C	A
				Control group 4	C	A	B
Control group 5	C	B	A

TABLE 7 quality testing of different combinations of adjuvants

From the test results of table 7, it can be seen that: compared with 5 control groups, the preparation prepared by the experimental group (namely the root bactericide) has the best indexes, the highest suspension rate, excellent water dispersibility, pourability, water resistance and the like, and the performance of the preparation is superior to that of other control groups.

Efficacy verification example 8: prevention and treatment effect of finished preparation on southern blight

The ratio of the bactericide for the root of the fruit tree seedling (volume mL) prepared in example 4 to the peanut seeds (mass) is 1:25, 1:50 and 1:100, the blank control is carried out by using clear water, the control is carried out by using 2.5g/L pyraclostrobin suspending agent, the medicine seed ratio is 1:100, and 9 peanut seeds are treated each time. Selecting uniform and plump peanut seeds, uniformly stirring the seeds and the medicament to uniformly attach the medicament to the surfaces of the seeds, spreading the seeds, airing the seeds, and sowing the seeds in a flowerpot with the diameter of 15 cm. During sowing, the turfy soil is filled into 3/4 deep in a flowerpot, then peanut seeds are uniformly sown, a layer of turfy soil is sprayed, barley grains with southern blight bacteria are inoculated, and finally a layer of thin soil is sprayed. After sowing, the flowerpot is placed in a light incubator, light and dark alternate (12:12) cultivation is carried out for 15 days at the temperature of 25 ℃, the disease condition of each seedling is observed, and the prevention and treatment effect of the pesticide is calculated.

Disease severity was graded on a scale of 0-4:

level 0: the plant is asymptomatic, and no lesion spots are visible at the stem;

level 1: the disease spots are generated only at the base of the stem, and the area of the disease spots accounts for below 1/5 of the whole plant;

and 2, stage: the stem base generates a constriction symptom, the disease spot area accounts for 1/5-1/3 of the whole plant, and the whole plant shows wilting, withering or death and the like;

and 3, level: the lesion area accounts for 1/3-2/3 of the whole plant, and the whole plant is withered or dead;

4, level: the lesion area is more than 2/3 of the whole plant, and the whole plant dies.

The calculation formula of the disease index and the prevention and treatment effect is as follows:

disease index (%) ═ Σ (number of diseased plants at each stage × the disease level value)/(total number of investigated plants × highest level value) × 100;

the preventing and treating effect (%) is (contrast disease index-treatment disease index)/contrast disease index x 100.

Table 8: prevention and treatment effect of fruit tree seedling root bactericide on peanut southern blight

The control effect of the medicament is shown in table 8. From the results of table 8, it can be seen that: the root treatment agent provided in example 4 has a better control effect on the control effect of the southern blight of peanuts, has an obvious control effect compared with a control, and is also higher than the control effect of 2.5g/L pyraclostrobin seed coating agent. By further experiments we obtained: the root treatment agents of examples 5 to 6 also had control effects on southern blight, which were slightly inferior to example 4 but higher than the control group.

And when the seed ratio of the preparation to the fruit tree seedling root bactericide is 1:25, the fruit tree seedling root bactericide has a relatively ideal prevention and control effect on the sclerotium rolfsii pathogenic bacteria, and the prevention and control effect reaches 88 percent, which shows that the fruit tree seedling root bactericide has a relatively good prevention and control effect on the sclerotium rolfsii of the peanut root, and can be used for prevention and control of the sclerotium rolfsii of the peanut.

It should be understood that the technical solutions and concepts of the present invention may be equally replaced or changed by those skilled in the art, and all such changes or substitutions should fall within the protection scope of the appended claims.

Claims (8)

1. The fruit tree seedling root bactericide compounded by tolclofos-methyl and pyraclostrobin is characterized by comprising the following components in percentage by mass: 3.9-35% of effective bactericidal component, 0.01-0.5% of plant growth regulator, 0.25-1.0% of thickening agent, 6.0-12.0% of wetting dispersant, 7.0-13.0% of filler, 0.15-0.5% of film-forming agent, 0.05-0.2% of acid-base regulator and 0.25-1% of defoaming agent; the solvent is water; the mass ratio of tolclofos-methyl to pyraclostrobin is 45: 2; wherein the plant growth regulator is 6-benzylaminopurine; the wetting dispersant is a mixture of SP-2728 and SP-SC 29; the thickening agent is sodium carboxymethyl cellulose; the filler is kaolin and the film forming agent is sodium silicate.

2. The fruit tree seedling root bactericide as claimed in claim 1, further comprising: 2.5-7.5% of an antifreezing agent, wherein the antifreezing agent is one or more of ethanol, glycerol, urea and sodium chloride; 0.025-0.1% of preservative 1, 2-benzisothiazolin-3-one.

3. The fruit tree seedling root bactericide as claimed in claim 1, further comprising a warning color in an amount of 0.025-0.1%.

4. The fruit tree seedling root bactericide as claimed in claim 1, further comprising a nutrient substance in an amount of 0.5-2.0%, wherein the nutrient substance is sucrose, glucose or maltose.

5. The fruit tree seedling root bactericide as claimed in claim 1, which is mainly composed of the following components in parts by mass:

11.25% of tolclofos-methyl, 0.5% of pyraclostrobin, 8.0% of compound wetting dispersant, 0.5% of sodium carboxymethylcellulose, 10.0% of kaolin, 0.25% of sodium silicate, 5.0% of urea, 0.05% of neutral black, 0.1% of citric acid, 0.05% of 6-BA, 0.05% of 1, 2-benzisothiazolin-3-one, 0.5% of organic silicon, 1.0% of cane sugar and the balance of water; wherein the compound wetting dispersant is a mixture of SP-2728 and SP-SC29 with the mass ratio of 5: 3.

6. The preparation method of the fruit tree seedling root bactericide compounded by tolclofos-methyl and pyraclostrobin as claimed in claim 1, is characterized by comprising the following steps:

1) uniformly mixing the effective bactericidal component, the filler, the wetting dispersant, the plant growth regulator, the thickening agent and the film forming agent, adding 40-50% of the total water, performing primary sanding, and treating for 30-60 min;

2) then adding warning color, antifreezing agent and 20-30% of the total water amount, and performing secondary sanding for 30 min;

3) finally, adding a defoaming agent, an acid-base regulator, a preservative, nutrient substances and the rest water, and performing sanding for the third time for 60 min;

4) separating the sand from the sand medium, shearing and emulsifying for 10min with a shearing machine to obtain a preparation; and after the quality inspection is qualified, the bactericide for the root of the fruit tree seedling is obtained.

7. The use method of the bactericide for the root of the fruit tree seedling as claimed in claim 1, wherein the bactericide for the root of the fruit tree seedling is diluted to 25-150 times of the liquid medicine by water when the seedling is treated, and the root of the fruit tree seedling is planted with the liquid medicine after being soaked in the liquid medicine for 30-60 min;

when treating seeds, the bactericide for the roots of the fruit tree seedlings is mixed with the seeds according to the mass ratio of 1:25-50, a small amount of water is added to prepare a medicament, the medicament is uniformly attached to the surfaces of the seeds, and the seeds are aired for sowing.

8. The application of the fruit tree seedling root bactericide according to claim 1 in preventing and treating fruit tree seedling root diseases.