CN116784328A

CN116784328A - Composition containing biological source bactericide and application thereof

Info

Publication number: CN116784328A
Application number: CN202310687260.XA
Authority: CN
Inventors: 彭成洲; 周学强; 周明松; 戴权; 王祥; 甄长征; 黄波
Original assignee: Yizhi Agricultural Technology Co ltd; Jiangxi Hongtudi Chemical Co ltd; South China University of Technology SCUT
Current assignee: Yizhi Agricultural Technology Co ltd; Jiangxi Hongtudi Chemical Co ltd; South China University of Technology SCUT
Priority date: 2023-06-12
Filing date: 2023-06-12
Publication date: 2023-09-22

Abstract

The invention discloses a composition containing a biological source bactericide and application thereof. The bactericidal composition comprises 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol and a biological source bactericide, wherein the biological source bactericide is one or more of kasugamycin, zhongshengmycin, ningnan mycin, polyoxin and natamycin. The bactericidal composition provided by the invention is used for preventing and treating agricultural diseases, namely, the pesticide contains 1-65wt.% of the bactericidal composition, and has obvious synergistic effect, and is mainly used for preventing and treating plant soft rot, plant black rot, plant canker and plant bacterial angular leaf spot.

Description

Composition containing biological source bactericide and application thereof

Technical Field

The invention relates to the technical field of pesticides, in particular to a composition containing a biological source bactericide and application thereof.

Background

The single bactericide variety is used for a long time, plant diseases are easy to generate drug resistance, the effect is poor in the field use process of the preparation, the defects of increased dosage, environment and agricultural product residues, increased dosage cost and the like are caused, and the application field of single preparation products is limited. In the aspect of agricultural disease control, the compounding of pesticides is an important means for delaying and solving the problem of pathogen drug resistance. The pesticide compound composition with the synergistic effect can enlarge the prevention spectrum, reduce the use dosage, reduce the environmental pollution and cause less resistance to pathogens.

Biopesticide refers to a pesticide produced by using a naturally occurring active substance produced by living organisms or a living organism itself, and chemical derivatives of naturally occurring active substances and the like are sometimes referred to as biopesticides. Along with the development of society and economy, ecological consciousness of people is continuously enhanced, and problems such as environmental pollution and the like caused by long-term use of chemical pesticides are more widely focused, and biological pesticides are rapidly developed due to the characteristics of environmental friendliness and the like, so that the biological pesticides become an important direction for future pesticide development.

CN107616178A discloses a composition containing ZJ10520 and a biogenic bactericide, which consists of a first active ingredient, a second active ingredient and a third active ingredient. The first active ingredient is ZJ10520; the second active ingredient is a biological source bactericide, and is at least one selected from validamycin, ningnanmycin, polyoxin, zhongshengmycin, bacillus subtilis, ethylicin, oligosaccharin and osthole; the third active ingredient is at least one selected from triazole bactericides, imidazole bactericides, oxazole bactericides, amide bactericides, dicarboximide bactericides, thiazole bactericides, pyrrole bactericides, morpholine bactericides, pyridine bactericides, pyrimidine bactericides, quinoline bactericides, organophosphorus bactericides, methoxy acrylic ester bactericides, carbamate bactericides and antibiotic bactericides. Can be used for preventing and treating rice sheath blight, rice damping-off, false smut, melon damping-off, early blight of tomato, strawberry gray mold, powdery mildew of cucumber, bacterial angular leaf spot of cucumber, cabbage soft rot, tomato bacterial wilt, watermelon damping-off, tobacco virus disease, cotton damping-off, wheat sheath blight, potato black nevus disease, or any one of the following diseases of wheat, vegetables and fruits: powdery mildew, black spot, rust, scab, anthracnose, damping off, gray mold, smut, leaf spot, downy mildew, sclerotinia, fusarium wilt, bakanae disease, and scab.

CN113396937a discloses a composition of multiple enzymes and biological bactericides, which has obvious synergistic effect after compounding, reduces the dosage, delays the generation of drug resistance and has the effects of increasing yield and improving efficiency by one or more of the multiple enzymes and the biological bactericides. The composition is mainly used for preventing and treating tobacco virus diseases, tomato late blight, cotton verticillium wilt, rice blast and the like, and has better prevention and treatment effects on cabbage soft rot, cucumber bacterial angular leaf spot, kiwi fruit canker, citrus canker and the like.

At present, a sterilizing composition compounded by 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol and a biological source bactericide is mainly used for preventing and treating cabbage soft rot, cabbage black rot and citrus canker in agricultural diseases, and the prior art has not been reported.

Disclosure of Invention

In view of the above-mentioned defects of the prior art, the technical problem to be solved by the invention is to provide a bactericidal composition which has reasonable components, obvious synergistic effect and safety to crops, is applied to preventing and treating agricultural diseases, and is mainly used for preventing and treating soft rot, black rot, ulcer and bacterial angular leaf spot.

In order to achieve the above object, the present invention provides a bactericidal composition comprising 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol and a biogenic bactericide;

the structure of the 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol is shown as a formula I:

wherein:

r in the structural formula I ₁ 、R ₂ Each independently H, C _1-12 An alkanyl group;

r in the structural formula I ₃ 、R ₄ Each independently H, C _1-4 An alkanyl group.

Preferably, the weight ratio of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol to the biogenic bactericide in the bactericidal composition is 1:50-50:1. More preferably, the weight ratio of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol to the biogenic bactericide is from 1:20 to 20:1.

Preferably, the biological source bactericide is at least one of kasugamycin, mesogenic fungi, ningnanmycin, polyoxin and natamycin bactericides.

More specifically, the invention also provides application of the bactericidal composition containing 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol in preparing pesticides. Specifically, the above-described fungicidal composition is contained in an amount of 1 to 65wt.% in a pesticide.

Preferably, the pesticide is one of emulsifiable concentrate, microemulsion, aqueous emulsion, suspoemulsion, dispersible oil suspending agent, wettable powder and water dispersible granule.

Preferably, the pesticide is in the form of a microemulsion, and comprises the following components: 0.1-40wt.% of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol, 0.1-15wt.% of biological source bactericide, 8-20wt.% of emulsifier, 0.1-10wt.% of stabilizer, 0.1-20wt.% of synergist and the balance of water.

Preferably, the pesticide is in the form of an aqueous emulsion and comprises the following components: 0.1-40wt.% of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol, 0.1-10wt.% of a biogenic bactericide, 0-10wt.% of a solvent, 0.1-5wt.% of an emulsifying agent, 0.1-5wt.% of a wetting agent, 0.1-15wt.% of a dispersing agent, 0.1-10wt.% of a stabilizing agent, 0.1-20wt.% of a synergist and the balance of water.

The disease prevention and control of the pesticide is plant soft rot, plant black rot, plant canker and plant bacterial angular leaf spot.

Among the pesticides are, but are not limited to, solvents, emulsifiers, wetting agents, stabilizers, synergists, dispersants, adhesion agents, acid-base modifiers, preservatives; are all known substances and are all common auxiliary agents in pesticide preparations.

The solvent is one or a mixture of any of water, methanol, ethanol, acetone, dimethylbenzene, n-butanol, ethyl acetate, cyclohexanone, petroleum ether, benzene, toluene, carbon tetrachloride and chloroform in any proportion; preferably water, methanol, n-butanol, xylene, cyclohexanone.

The emulsifier is one or a mixture of any several of sodium dodecyl benzene sulfonate, sodium dodecyl polyoxyethylene ether sulfate, cetyl trimethyl ammonium bromide, octyl phenol polyoxyethylene ether, polyvinyl alcohol, alkylphenol polyoxyethylene ether OP-10, pesticide emulsion 700#, pesticide emulsion 2201#, pesticide emulsion 33#, fatty alcohol polyoxyethylene ether AEO-9, alkylphenol formaldehyde resin polyoxyethylene ether, calcium dodecyl benzene sulfonate, castor oil polyoxyethylene ether, ethylans-500 LQ, sodium diisooctyl succinate and nonylphenol polyoxyethylene (EO=10) ether phosphate in any proportion; preferably alkylphenol ethoxylates OP-10, nongru 700#, nongru 2201#, nongru 33#, calcium dodecylbenzenesulfonate, tristyrylphenol ethoxylate 602#, castor oil ethoxylate, ethylans-500 LQ, sodium diisooctyl sulfosuccinate, EO-PO block polyether, fatty alcohol polyoxyethylene ether AEO-9, nonylphenol polyoxyethylene (EO=10) ether phosphate.

The wetting agent is one or a mixture of several of EO-PO block polyether, rosin-based vegetable oil ND-45, lutensol TO8, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, sodium dodecyl sulfate and Terwet1004 in any proportion; preferably one or a mixture of any of EO-PO block polyether, rosin-based vegetable oil ND-45, alkylphenol ethoxylate OP-10 and sodium dodecyl sulfate in any proportion.

The stabilizer is preferably one or a mixture of more than one of Ethylan NS-500LQ, phenyl salicylate, epichlorohydrin, epoxidized soybean oil, antioxidant BHT, glacial acetic acid and citric acid in any proportion.

The synergistic agent is one or a mixture of any several of di-sec-octyl maleate sodium sulfonate, lutensol TO8, alkylphenol ethoxylates, fatty alcohol ethoxylates, sodium dodecyl alcohol ether sulfate, polyoxyethylene sorbitan fatty acid ester, alkylaryl ether group glycerol phthalate, methyl esterified vegetable oil and mineral oil in any proportion; preferably, the synergistic agent is one or a mixture of any of sodium di-sec-octyl maleate sulfonate, lutensol TO6 and Lutensol TO8 in any proportion.

The synergistic agent can be directly added into the preparation, and can also be used as a tank mixing auxiliary agent to be added when being used in the field.

The application method of the pesticide in the application is any one of soil application, stem and leaf spraying, fumigation, irrigation, drip irrigation, atomization, gasket release, powder spraying, mucus tape release, trunk smearing and bait release; preferably stem and leaf spray.

The stem and leaf spray can directly act on the hazard parts of plant diseases and insect pests and grass pests, and the control effect is quick; the dosage of the medicine can be reduced, because the medicine effect of the spray on the leaf surface can be exerted more fully, compared with the application of the medicine to the soil, the dosage of the medicine and the pollution of the pesticide to the soil and the environment can be reduced; spraying can be performed according to the growth requirement of crops, and the application time and the dosage can be flexibly controlled; effectively controlling the plant diseases and insect pests and grass pests of leaf surfaces and stems.

The application dosage of the bactericidal composition provided by the invention is flexible, can be changed according to control objects, and the external conditions, especially the application temperature, humidity and dosage forms of additives can be changed within a wider range, and the dosage of the active ingredients of the bactericidal composition is 0.1-2000 g/ha, preferably 0.1-500 g/ha, more preferably 100-300 g/ha.

The invention has the beneficial effects that:

1. the invention aims to provide a composition containing 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol and a biological source bactericide and application thereof, wherein the composition has remarkable synergistic effect on preventing and treating agricultural diseases after the 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol and the biological source bactericide are mixed, and the biological source bactericide can be one or more of kasugamycin, mesogenic fungi, ningnanmycin, polyoxin and natamycin.

2. The 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol in the bactericidal composition has better chemical stability and the heat storage degradation rate is lower than 5 percent.

3. In the stabilizer, the antioxidant BHT and the phenyl salicylate have the main functions of antioxidation and photolysis, and can play the roles of the stabilizer, the antioxidant and the photodegradation agent at the same time when being used for preventing and treating agricultural diseases.

4. The bactericidal composition containing 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol provided by the invention is applied to crops, and can effectively prevent and treat plant soft rot, plant black rot, plant canker and plant bacterial angular leaf spot.

5. The sterilization composition provided by the invention has flexible application dosage, can be changed according to control objects, can change external conditions, especially the application temperature, humidity and dosage forms of additives within a wider range, and has the effective component dosage of 0.1-500 g/hectare or more, preferably has the effective component dosage of 100-300 g/hectare.

Detailed Description

Test example 1

In general, three types of action are exhibited after pesticides are mixed: additive action, synergistic action and antagonistic action. In order to prevent and treat soft rot and black rot in agricultural production, a compound synergistic study is carried out by using 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol and kasugamycin, and a specific test method is as follows.

1. Combined toxicity determination of sterilizing composition on soft rot and black rot of cabbages

The test subjects were cabbage soft rot pathogen (Erwinia carotovora pv. Carotovora) and cabbage black rot pathogen (Xanthomonas campestris pv. Campestris). Reference is made to "pesticide biological Activity evaluation SOP", biometric test guidelines NY/T1156.16-2008 and pesticide indoor biometric test guidelines NY/T1156.6-2006. The toxicity measurement results of the bactericidal composition of the invention on white vegetable soft rot are shown in table 1, the toxicity measurement results of the bactericidal composition on white vegetable black rot are shown in table 2, and the toxicity measurement results of the bactericidal composition on citrus canker are shown in table 3. Wherein 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol is abbreviated as alkyl benzenediol in the table.

(1) Turbidity testing method

Adopting turbidity method to dilute the Chinese cabbage soft rot and black rot bacteria grown on NA slant culture medium into 1×10 with sterile water ⁷ Suspension with CFU concentration, 100 mu L of suspension is sucked by a pipette and added into NB culture medium containing liquid medicines with different concentrations, the inoculated NB culture medium is placed at 28 ℃ for shaking (120 r/min) culture, and 4 times of repetition are carried out on each treatment. Measuring turbidity of each treatment before starting culture, measuring and recording turbidity of each treatment when control treatment reaches logarithmic phase, A ₀ For the blank, the turbidity is increased by A ₁ The turbidity increase is treated with the agent.

(2) Inhibition of bacterial growth

The investigation data calculate the bacterial growth inhibition rate according to a formula, the bacteriostasis rate result is expressed in percent (%), and the calculated result retains two decimal places. The bacterial growth inhibition rate was calculated as follows:

P＝{(A ₀ -A ₁ )/A ₀ }×100％

wherein:

p-growth inhibition;

A ₀ -increase in turbidity of the blank;

A ₁ -the turbidity increase by the agent treatment.

(3) Co-toxicity coefficient

According to the bacteriostasis rate result, solving a virulence regression equation and EC ₅₀ Value, EC ₅₀ The value is a standard medicament, namely a medicament safety index, and 50% of individuals die or are poisoned only by increasing the effective dose of 50% of individuals by more than two times, and the larger the value is, the safer the medicament is relatively; in general, three types of action are exhibited after pesticides are mixed: additive action, synergistic action and antagonistic action. The combined action type of the two medicinal active ingredients with different mixing ratios is evaluated according to the grand cloud Pei co-toxicity coefficient method (CTC): the co-toxicity coefficient is greater than 120, which indicates that the synergistic effect is achieved; if less than 80, antagonism is indicated; between 80 and 120, indicated as additive.

Measured virulence index (ATI) = (standard agent EC ₅₀ Test agent EC ₅₀ )×100

Theoretical virulence index (TTI) =percentage of agent a in ATI x mix + percentage of agent B in ATI x mix

Co-toxicity coefficient (CTC) = (blend ATI/blend TTI) ×100

TABLE 1 determination of Chinese cabbage Soft rot Virus results

From Table 1, it can be seen that the weight ratio of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol to kasugamycin is in the range of 8:1-1:10, and the co-toxicity coefficient of the kasugamycin to white vegetable soft rot pathogens is greater than 120, which indicates that the mixing of the two components in the range shows remarkable synergistic effect. Wherein, when the weight ratio of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol to kasugamycin is 4:1-1:6, the co-toxicity coefficient to soft rot is more than 150, the synergistic effect is most obvious, and when the weight ratio of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol to kasugamycin is 1:1, the co-toxicity coefficient to white vegetable soft rot is 181.67, which indicates that the synergistic effect of the ratio is most obvious.

TABLE 2 determination of the black rot Virus strength of Chinese cabbage

Medicament treatment	EC ₅₀ (mg/L)	CTC
			Alkyl benzene diphenol (A)	8.75	-
Zhongshengmycin (B)	18.31	-
			A:B＝50：1	20.46	43.23
A:B＝40：1	15.81	56.10
			A:B＝30：1	14.32	62.21
A:B＝20：1	13.64	65.88
			A:B＝10：1	11.82	77.94
A:B＝8：1	11.61	80.30
			A:B＝6：1	10.72	88.62
A:B＝4：1	8.98	123.27
			A:B＝2：1	6.63	161.77
A:B＝1：1	7.21	194.70
			A:B＝1：2	7.43	186.46
A:B＝1：4	8.96	175.04
			A:B＝1：6	9.45	175.92
A:B＝1：8	10.58	162.55
			A:B＝1：10	12.25	143.54
A:B＝1：20	16.78	110.08
			A:B＝1：30	20.96	89.73
A:B＝1：40	23.21	81.80
			A:B＝1：50	25.05	76.23

From Table 2, it can be seen that the weight ratio of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol to Zhongshengmycin is in the range of 2:1-1:10, and the co-toxicity coefficients of the two components to black rot germs are all greater than 120, which indicates that the mixing of the two components in the range shows remarkable synergistic effect. Wherein, when the weight ratio of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol to the Zhongshengmycin is 2:1-1:8, the co-toxicity coefficient to pathogenic bacteria of black rot is more than 150, the synergistic effect is most obvious, and when the weight ratio of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol to the Zhongshengmycin is 1:1, the co-toxicity coefficient to pathogenic bacteria of black rot is 194.70, which indicates that the ratio synergistic effect is most obvious.

2. Combined determination of the compounding of a fungicidal composition for citrus canker

The test subjects were citrus canker pathogens (Xanthomonas campestris pv. Citri). Adopts a bacteriostasis circle method: culturing the bacteria to be tested on a culture medium for 40h, adding sterile water to scrape the lawn to prepare a bacterial solution, adding 1mL of the bacterial solution into a sterile petri dish, pouring 10mL of melted NT culture medium with the liquid temperature of 10-50 ℃, placing a sterilized oxford cup in the center of a flat plate, taking 100 mu L of liquid medicine, dripping the liquid medicine into the oxford cup, and repeating the treatment for 4 times each time, wherein sterile water treatment is used as a control. The dishes were incubated at 26℃for 48h, and the diameter (mm) of the zone of inhibition was measured and recorded.

According to the bacteriostasis rate result, solving a virulence regression equation and EC ₅₀ Value, EC ₅₀ The value is a standard medicament, namely a medicament safety index, and 50% of individuals die or are poisoned only by increasing the effective dose of 50% of individuals by more than two times, and the larger the value is, the safer the medicament is relatively; the combined action type of the two medicinal active ingredients with different mixing ratios is evaluated according to the grand cloud Pei co-toxicity coefficient method (CTC): if the co-toxicity coefficient is greater than 120, the synergy is shown; if less than 80, antagonism is indicated; between 80 and 120, indicated as additive.

Co-toxicity coefficient (CTC) = (blend ATI/blend TTI) ×100

TABLE 3 determination of citrus ulcer virulence

From Table 3, it can be seen that the weight ratio of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol to kasugamycin is in the range of 40:1-1:20, and the co-toxicity coefficient for ulcer is greater than 120, which indicates that the mixing of the two components in the range shows remarkable synergistic effect. Wherein, when the weight ratio of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol to kasugamycin is 8:1-1:10, the co-toxicity coefficient to pathogenic bacteria of ulcer is more than 150, the synergistic effect is most obvious, and when the weight ratio of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol to kasugamycin is 4:1, the co-toxicity coefficient to pathogenic bacteria of ulcer is 199.71, which indicates that the synergistic effect of the ratio is most obvious.

Example 1

The preparation method of the pesticide containing 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol and kasugamycin (the dosage form is aqueous emulsion) comprises the following steps:

60g of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol, 30g of kasugamycin, 24g of calcium dodecyl benzene sulfonate, 76g of tristyrylphenol polyoxyethylene ether 602#, 5g of antioxidant BHT, 1g of glacial acetic acid and 120g of methanol are weighed, water is added to be added to 1000g of the mixture, the mixture is uniformly mixed at room temperature, and high-speed shearing and emulsification are carried out to prepare 9wt.% of the aqueous emulsion containing 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol kasugamycin.

Example 2

The preparation method of the pesticide (the dosage form is an aqueous emulsion) containing 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol and the Zhongshengmycin comprises the following steps:

60g of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol, 60g of Zhongshengmycin, 45g of emulsifier 33#, 15g of Ethylans-500 LQ, 40g of di-sec-octyl maleate sodium sulfonate, 15g of antioxidant BHT, 0.8g of glacial acetic acid and 120g of cyclohexanone are weighed, water is added to 1000g, the mixture is uniformly mixed at room temperature, and high-speed shearing emulsification is carried out to prepare the aqueous emulsion containing 12wt.% of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol.

Example 3

The preparation method of the pesticide (the dosage form is an aqueous emulsion) containing 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol and kasugamycin comprises the following steps:

50g of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene, 50g of kasugamycin, 40g of sodium di-sec-octyl maleate sulfonate, 45g of pesticide emulsion 33#, 15g of Ethylans-500 LQ, 15g of antioxidant BHT, 30g of epoxidized soybean oil and 120g of cyclohexanone are weighed, water is added to 1000g, the mixture is uniformly mixed at room temperature, and high-speed shearing and emulsification are carried out to prepare 10wt.% of water emulsion containing 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol and kasugamycin.

Example 4

The preparation method of the pesticide (the dosage form is microemulsion) containing 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol and kasugamycin comprises the following steps:

60g of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene, 30g of kasugamycin, 20g of alkylphenol polyoxyethylene OP-10, 24g of calcium dodecyl benzene sulfonate, 100g of xylene, 1g of monoethanolamine and 120g of methanol are weighed, water is added to 1000g of the mixture, the mixture is uniformly mixed at room temperature, and high-speed shearing and emulsification are carried out to prepare 9wt.% of microemulsion containing 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene kasugamycin.

Example 5

The preparation method of the pesticide (the dosage form is microemulsion) containing 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol and the Zhongshengmycin comprises the following steps:

60g of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol, 60g of Zhongshengmycin, 25g of alkylphenol polyoxyethylene OP-10, 35g of calcium dodecyl benzene sulfonate, 150g of xylene, 1g of monoethanolamine and 100g of methanol are weighed, water is added to 1000g of the mixture, the mixture is uniformly mixed at room temperature, and high-speed shearing and emulsification are carried out to prepare the microemulsion containing 12wt.% of the 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol.

Example 6

50g of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene, 50g of kasugamycin, 40g of nonylphenol polyoxyethylene (EO=10) ether phosphate, 40g of agricultural emulsion 700#, 20g of agricultural emulsion 2201#, 20g of epichlorohydrin, 5g of sodium chloride, 30g of cyclohexanone, 6g of polyvinyl alcohol and 4g of sodium benzoate are weighed, water is added to 1000g, the mixture is uniformly mixed at room temperature, and high-speed shearing emulsification is carried out to prepare 10wt.% of microemulsion containing 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene kasugamycin.

Example 7

100g of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene, 25g of kasugamycin, 30g of calcium dodecyl benzene sulfonate, 20g of castor oil polyoxyethylene ether, 50g of tristyrylphenol polyoxyethylene ether 602# and 50g of cyclohexanone are weighed, water is added to be added to 1000g, the mixture is uniformly mixed at room temperature, and high-speed shearing emulsification is carried out to prepare 12.5wt.% of water emulsion containing 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene kasugamycin.

Example 8

100g of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene, 50g of kasugamycin, 60g of fatty alcohol polyoxyethylene ether AEO-9, 20g of ethyllanNS-500 LQ, 8g of phenyl salicylate, 1.5g of citric acid, 15g of LutensolTO8 and 50g of rosin-based vegetable oil ND-45 are weighed, water is added to 1000g, the mixture is uniformly mixed at room temperature, and high-speed shearing emulsification is carried out to prepare 15wt.% of an aqueous emulsion containing 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene kasugamycin, namely the pesticide containing 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene.

Example 9

100g of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene, 25g of kasugamycin, 30g of EO-PO block polyether, 80g of castor oil polyoxyethylene ether, 30g of diisooctyl sodium sulfonate succinate, 50g of n-butanol and 100g of cyclohexanone are weighed, water is added to 1000g of cyclohexanone, the mixture is uniformly mixed at room temperature, and high-speed shearing emulsification is carried out to prepare the microemulsion containing 12.5wt.% of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene kasugamycin.

Example 10

100g of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene, 50g of kasugamycin, 200g of DYAY-03, 40g of tristyrylphenol polyoxyethylene ether 602#, 150g of methanol, 50g of n-butanol and 100g of cyclohexanone are weighed, water is added to be added to 1000g, the mixture is uniformly mixed at room temperature, and high-speed shearing and emulsification are carried out to prepare a microemulsion containing 15wt.% of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene kasugamycin.

The amounts of the above examples 1 to 10 added are shown in Table 4, wherein 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol is abbreviated as alkylbenzenediol in the table.

Table 4 summary of the amounts added in examples

	Medicament A	Medicament B	Pesticide formulation	Ratio of A to B
					Example 1	Alkyl benzenediols	Kasugamycin	Aqueous emulsion	6wt.％：3wt.％
Example 2	Alkyl benzenediols	Zhongshengmycin	Aqueous emulsion	6wt.％：6wt.％
					Example 3	Alkyl benzenediols	Kasugamycin	Aqueous emulsion	5wt.％：5wt.％
Example 4	Alkyl benzenediols	Kasugamycin	Microemulsion preparation	6wt.％：3wt.％
					Example 5	Alkyl benzenediols	Zhongshengmycin	Microemulsion preparation	6wt.％：6wt.％
Example 6	Alkyl benzenediols	Kasugamycin	Microemulsion preparation	5wt.％：5wt.％
					Example 7	Alkyl benzenediols	Kasugamycin	Aqueous emulsion	10wt.％：2.5wt.％
Example 8	Alkyl benzenediols	Kasugamycin	Aqueous emulsion	10wt.％：5wt.％
					Example 9	Alkyl benzenediols	Kasugamycin	Microemulsion preparation	10wt.％：2.5wt.％
Example 10	Alkyl benzenediols	Kasugamycin	Microemulsion preparation	10wt.％：5wt.％

Test example 2

1. Chinese cabbage field efficacy test

The pesticide obtained by the preparation method of the examples 1-6 is subjected to a field efficacy test, and the soft rot disease grade, the incidence probability, the disease index and the prevention effect of the Chinese cabbage are counted.

The test is carried out in new town in Hanchuan city in Hubei province, and after the cabbage at the test point is transplanted, the medicine is sprayed once on days 15, 25, 35 and 45 respectively. The application method of the field pesticide effect test adopts a knapsack manual sprayer to carry out uniform spraying treatment on leaf surfaces, and the cultivation technology and other management measures in the growing period of the cabbages are carried out according to the conventional method.

The drug effect investigation method comprises the following steps: and (3) investigation of field disease occurrence at 35 days and 45 days after transplanting is performed by a full field investigation mode, and the number of disease plants and the number of disease stages are recorded, the disease index is calculated, and the control effect is corrected. Meanwhile, the safety of white vegetables in the test process, the influence on other organisms and unexpected events in the test process are observed and recorded, the disease grade, incidence probability, disease index and prevention effect of the cabbage soft rot are counted, and the field efficacy test result is shown in table 5, wherein 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol is called alkyl benzenediol in the table for short.

(1) Disease grade

The disease grade was rated 6 as follows:

level 0: no symptoms;

stage 1: the leaves are firstly seen as water stain-like brown speckles;

3 stages: the 1 st to 2 nd leaf base at the bottom has obvious disease spots;

5 stages: the outer leaves have 1/3-1/2 decay;

7 stages: the outer leaves are all rotten;

stage 9: the whole plant is rotten;

(2) Probability of onset

Incidence = number of lesions/investigation tree x 100%

(3) Index of disease condition

Disease index = (Σnumber of disease plants at each stage x representative value at each stage)/(total plant tree under investigation x representative value at highest disease stage) ×100

(4) Preventing effect

Control = (control disease index-treatment disease index)/(control disease index)

×100％

TABLE 5 cabbage field test results

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The first investigation was conducted on the 35 th day of the field test, and the comparison shows that the control effect of example 1, example 2, example 4 and example 6 on the cabbage soft rot is the highest, and is over 80%, which is obviously superior to other treatments. The control effect of the embodiment 3 and the embodiment 5 is lower than that of other medicament treatments, and the control effect is poor.

The second investigation is carried out on the 45 th day of the field test, and the comparison shows that the control effect of the examples 1-5 on the cabbage soft rot is the highest and is above 85%. The highest control effect of the example 4 is 90.55 percent, which is obviously superior to other treatments. The treatment prevention effect of the examples is higher than that of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene when used alone.

The data show that the 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol composition preparation provided by the invention can have better prevention and protection effects on white vegetable soft rot. In the test period, the cabbage does not have other obvious diseases except soft rot, and has no phytotoxicity symptoms, so that the sterilization composition provided by the invention is safe.

2. Citrus field efficacy test

The pesticides obtained by the preparation methods of examples 7-10 are subjected to field efficacy tests, and the canker disease grade, incidence probability, disease index and prevention effect of citrus are counted.

The test groups are arranged randomly, carried out simultaneously, and have consistent spraying quantity, and 5 spring bud points in the east, the south, the west, the north and the middle of each tree are marked before the medicine; each treatment was repeated 3 times, the blank was only applied with water, and the control was only applied with 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol.

The test is carried out in the Guangxi Zhuang autonomous region Nanning city in the Wu Qing dynasty region, the citrus trees with the tree age of 3-4 years are selected as test samples, the citrus is applied at the beginning of 3 months when the citrus is in the spring tip sprouting period, then the citrus canker disease prevention condition is counted after once every 15 days of continuous twice of application. The application method of the field pesticide effect test adopts a knapsack type manual sprayer to carry out uniform spraying treatment on leaf surfaces, and carries out positive and negative spraying on the leaf surfaces in the pesticide application process, wherein each pesticide treatment is carried out according to the water consumption of 2 kg per tree.

The drug effect investigation method comprises the following steps: the ulcer disease is investigated 14 days after the second application, the investigation is carried out by adopting a new tip leaf full investigation mode above the mark point, the total leaf number of the mark point leaf, the leaf number of each stage of disease and the disease progression are recorded, and the disease index and the correction control effect are calculated. Meanwhile, the safety of citrus trees, the influence on other organisms and unexpected events occurring in the test process are observed and recorded, the citrus canker disease grade, the incidence probability, the disease index and the control effect are counted, the field efficacy test results are shown in table 6, wherein 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol is called alkyl benzenediol in the table for short.

(1) Disease grade

The disease grade was rated 6 as follows:

level 0: the whole leaf has no disease spots;

stage 1: 1-3 lesions are formed on the leaf;

2 stages: 4-7 lesions are formed on the leaf;

3 stages: 8-11 lesions are formed on the leaf;

4 stages: more than 11 disease spots are arranged on the leaf blade;

5 stages: the diseased leaves fall off;

(2) Leaf disease rate

Disease leaf rate = number of diseased leaves/total number of investigated leaves x 100%

(3) Index of disease condition

Disease index = (Σnumber of attacks at each level×representative value at each level)/(total leaf number investigated×highest disease level) ×100

(4) Preventing effect

Control effect = (control disease index-treatment disease index)/(control disease index) ×100%

TABLE 6 results of citrus field efficacy tests

As can be seen from comparison of citrus field efficacy tests, the pesticide containing the 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol composition prepared in the embodiment 7-10 has good control effect on citrus canker, the control effect of the pesticide control treatment is over 90 percent, and the control effect is higher than that of the 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol when being singly used, which indicates that the compound use of the 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol and the biological source bactericide improves the bactericidal activity of the pesticide and can obviously reduce the use amount of the pesticide. The interval between preventive medicines is 15 days, which shows that the 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-dihydroxybenzene composition preparation provided by the invention can better protect citrus leaves during the period; the citrus trees grow well during the test period, and no phytotoxicity symptoms appear, which indicates that the sterilizing composition provided by the invention is safe to citrus.

Claims

1. A bactericidal composition, which is characterized by comprising 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol and a biological source bactericide;

wherein:

2. The bactericidal composition of claim 1 wherein: the weight ratio of the 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol to the biological source bactericide is 1:50-50:1.

3. The bactericidal composition of claim 2 wherein: the weight ratio of the 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol to the biological source bactericide is 1:20-20:1.

4. A bactericidal composition as claimed in any of claims 1 to 3 wherein: the biological source bactericide is at least one of kasugamycin, zhongshengmycin, ningnan mycin, polyoxin and natamycin bactericides.

5. Use of a fungicidal composition as claimed in any one of claims 1 to 4 for the preparation of pesticides.

6. The use according to claim 5, wherein: the pesticide contains 1-65wt.% of the bactericidal composition.

7. The use according to claim 5 or 6, wherein: the pesticide is one of emulsifiable concentrate, microemulsion, aqueous emulsion, suspoemulsion, dispersible oil suspending agent, wettable powder and water dispersible granule.

8. The use according to claim 7, wherein the pesticide is in the form of a microemulsion comprising the following components: 0.1-40wt.% of 3, 6-diisoalkyl cyclohexanone-4, 5-dialkyl-1, 2-benzenediol, 0.1-15wt.% of biological source bactericide, 8-20wt.% of emulsifier, 0.1-10wt.% of stabilizer, 0.1-20wt.% of synergist and the balance of water.

9. The use according to claim 7, wherein the pesticide is in the form of an aqueous emulsion comprising the following components: 0.1-40wt.% of 3, 6-diisoalkylcyclohexanone-4, 5-dialkyl-1, 2-benzenediol, 0.1-10wt.% of a biogenic bactericide, 0-10wt.% of a solvent, 0.1-5wt.% of an emulsifying agent, 0.1-5wt.% of a wetting agent, 0.1-15wt.% of a dispersing agent, 0.1-10wt.% of a stabilizing agent, 0.1-20wt.% of a synergist and the balance of water.

10. The use according to claim 5, wherein the disease to be controlled by the pesticide is soft rot, black rot, canker, bacterial angular leaf spot.