Succinate sulfonate-containing fungicide, and preparation method therefor and use thereof

Abstract

A succinate sulfonate-containing fungicide, and a preparation method therefor and a use thereof. The fungicide at least comprises the following components: (a) at least one chemically active substance for controlling crop fungal diseases, the chemically active substance being selected from one or more of tebuconazole, trifloxystrobin, prothioconazole, cyazofamid, cymoxanil, famoxadone, difenoconazole, pyraclostrobin, boscalid, and fludioxonil; (b) at least one succinate sulfonate; and (c) an auxiliary agent, the auxiliary agent comprising at least one of a carrier, a disintegrant, a binder, a rheology modifier, a dispersant, a wetting agent, a defoaming agent, a thixotropic agent, an antifreeze agent, a preservative, a thickener, a solvent, and an emulsifier. By optimizing a fungicide formulation system, the utilization rate of fungicidal agricultural active substances is improved, thereby achieving the objective of reducing dosage while enhancing efficacy; and the fungicide has high market promotion value.

Description

Fungicide containing succinate sulfonate and preparation method and application thereof TECHNICAL FIELD

[0001] The present application relates to the field of A01N47 / 00, in particular to a fungicide containing succinate sulfonate and preparation method and application thereof. BACKGROUND

[0002] Due to the change of planting structure, the rise of pathogen resistance, the long-term continuous use of single pesticide variety, the resistance of disease and the increase of use amount lead to the risk of cost increase, which also causes greater pollution to the environment. The prevention and treatment of diseases is becoming more and more difficult, and is facing great challenges. At present, the problem of drug resistance is mainly improved by screening different pesticide varieties and combining the compounds with significant synergistic effect. For example, Chinese patent CN107517982 A discloses a fungicidal composition containing thiazole zinc and bifenazate, which is used for preventing and treating bacterial diseases and fungal diseases of crops. Chinese patent (authorized publication number CN113243379B) discloses a fungicidal composition containing thiazolone and penconazole and its application, which is used for preventing and treating diseases such as pear black spot, grape white rot, apple anthracnose and pepper leaf spot, and has synergistic effect. Chinese patent (authorized publication number CN114766493B) discloses a fungicidal composition containing agricultural antibiotics and its application, which realizes the prevention and treatment of various plant fungal diseases by compounding fluazinam with polyoxin or Jinggangmycin A. However, the current fungicide has low utilization rate of active substance, and the amount of active ingredient needs to be added to a certain amount to achieve the corresponding prevention and treatment effect. Therefore, based on the comprehensive consideration of economy and environment, it is necessary to develop a reduced amount of synergistic preparation. SUMMARY

[0003] In order to solve the above problems, the present application provides a fungicide containing succinate sulfonate, which optimizes the formula system of fungicide, improves the utilization rate of fungicide agricultural active substance, achieves the purpose of reducing amount and increasing effect, and has high market promotion value.

[0004] In one aspect, the present application provides a fungicide containing succinate sulfonate, which at least comprises the following components:

[0005] (a) at least one chemical active substance for preventing and treating fungal diseases of crops, the chemical active substance is selected from one or more of tebuconazole, trifloxystrobin, prothioconazole, cyazofamid, cymoxanil, famoxadone, difenoconazole, pyraclostrobin, boscalid and fludioxonil;

[0006] (b) at least one succinate sulfonate, the succinate sulfonate has the structure shown in formula (1): formula (1)

[0007] wherein R1, R2 are both C6-C 12 alkyl;

[0008] (c) an adjuvant comprising at least one of a carrier, a disintegrant, a binder, a rheological agent, a dispersant, a wetting agent, an antifoaming agent, a thixotropic agent, an antifreezing agent, a preservative, a thickening agent, a solvent, an emulsifier.

[0009] The content of the chemical active substance is 10-40% by mass percentage, the content of the succinate sulfonate is 0.5-5%, and the adjuvant makes up the balance.

[0010] As a preferred technical solution, R in the formula (1) is C6-C8 alkyl, preferably any one of the following structures: -(CH2)5CH3, -CH2CH (CH3), (CH2)2CH3, -CH2CH (C2H5) CH2CH3, -(CH2)7CH3, -CH (CH3) (CH2)5CH3, -CH2CH (C2H5) (CH2)3CH3. 2

[0011] As a preferred technical solution, the formula (1) is obtained by reacting succinic acid and alkyl ester, and the mass percentage of the alkyl ester in the formula (1) is 30-80%, preferably 50-70%.

[0012] As a preferred technical solution, the succinate sulfonate is selected from at least one of sodium di-n-hexyl succinate sulfonate, sodium di-2-methyl pentyl succinate sulfonate, sodium di-2-ethyl butyl succinate sulfonate, sodium di-n-octyl succinate sulfonate, sodium di-sec-octyl succinate sulfonate, and sodium di-iso-octyl succinate sulfonate. Preferably, it is one of sodium di-n-hexyl succinate sulfonate, sodium di-2-methyl pentyl succinate sulfonate, sodium di-n-octyl succinate sulfonate, sodium di-sec-octyl succinate sulfonate, and sodium di-iso-octyl succinate sulfonate.

[0013] As a preferred technical solution, the dosage form of the fungicide containing succinate sulfonate is one of a suspension concentrate, an emulsifiable concentrate, a granule, a wettable powder, and a water dispersible granule, preferably one of a suspension concentrate, a water dispersible granule, and an emulsifiable concentrate.

[0014] As a preferred technical solution, the dosage form of the fungicide containing succinate sulfonate is a suspension concentrate, and the preparation raw materials thereof at least include 20-40% of a chemical active substance, 2-8% of a wetting agent, 2-6% of a dispersant, 3-5% of a succinate sulfonate, 0.1-1% of an antifoaming agent, 0.5-2% of a thixotropic agent, 0.1-0.3% of a thickening agent, 3-6% of an antifreezing agent, 0.05-0.2% of a preservative, and deionized water making up the balance. ​

[0015] As a preferred technical solution, the chemical active substance is at least two of tebuconazole, trifloxystrobin, prothioconazole, boscalid, fludioxonil, difenoconazole, pyraclostrobin. Preferably, the chemical active substance is one of tebuconazole, trifloxystrobin combination, prothioconazole, trifloxystrobin combination, boscalid, fludioxonil combination, difenoconazole, pyraclostrobin combination.

[0016] Preferably, the mass ratio of tebuconazole and trifloxystrobin is (1.8-2.5):(0.6-1), preferably 2:1.

[0017] Preferably, the mass ratio of prothioconazole and trifloxystrobin is (2-3):(0.6-1), preferably 2.5:1.

[0018] Preferably, the mass ratio of boscalid and fludioxonil is (2-3):(0.6-1), preferably 2.4:0.6.

[0019] Preferably, the mass ratio of difenoconazole and pyraclostrobin is (1.8-2.5):(0.6-1), preferably 2:1.

[0020] Preferably, the wetting agent is at least one of alkylphenol polyoxyethylene ether phosphate, styrene-maleic anhydride random copolymer, fatty alcohol polyoxyethylene ether sulfate, triphenyl ethylene phenol polyoxyethylene ether sulfate ammonium salt.

[0021] Preferably, the dispersing agent is at least one of EO-PO block copolymer, naphthalene sulfonate formaldehyde condensate, styryl phenol polyoxyethylene polyoxypropylene ether.

[0022] Preferably, the succinate sulfonate is one of diisooctyl succinate sodium sulfonate, di-n-hexyl succinate sodium sulfonate, di-sec-octyl succinate sodium sulfonate, di-2-methyl pentyl succinate sodium sulfonate.

[0023] Preferably, the defoaming agent is at least one of high carbon alcohol, organosilicon, polyether, mineral oil, silicon polyether, preferably organosilicon defoaming agent SAG1522.

[0024] Preferably, the thixotropic agent is silicon dioxide and / or magnesium aluminum silicate.

[0025] Preferably, the thickening agent is xanthan gum.

[0026] Preferably, the antifreeze agent is propylene glycol and / or ethylene glycol.

[0027] Preferably, the preservative is isothiazolinone.

[0028] Preferably, the solvent is deionized water.

[0029] As a preferred technical solution, the dosage form of the succinate sulfonate-containing fungicide is an emulsifiable concentrate, and the preparation raw materials thereof include, in terms of mass percentage, at least 20-30% of a chemical active substance, 10-30% of an emulsifier, 3-5% of a succinate sulfonate, and the balance of an organic solvent.

[0030] Preferably, the chemical active substance is pyraclostrobin.

[0031] Preferably, the emulsifier is at least one selected from calcium dodecylbenzenesulfonate, alkylphenol polyoxyethylene ether, and fatty alcohol polyoxyethylene ether, and preferably, the emulsifier is a combination of calcium dodecylbenzenesulfonate and triphenylethyl phenol polyoxyethylene ether, and the mass ratio of the calcium dodecylbenzenesulfonate to the triphenylethyl phenol polyoxyethylene ether is (10-15):(5-10), preferably 11:9.

[0032] The succinate sulfonate is at least one selected from sodium di-n-octyl succinate sulfonate, sodium di-sec-octyl succinate sulfonate, and sodium di-iso-octyl succinate sulfonate, and preferably, the succinate sulfonate is sodium di-n-octyl succinate sulfonate.

[0033] The organic solvent is preferably N,N-dimethyl decanamide.

[0034] As a preferred technical solution, the dosage form of the succinate sulfonate-containing fungicide is a water dispersible granule, and the preparation raw materials thereof include, in terms of mass percentage, at least 10-30% of a chemical active substance, 2-6% of a wetting agent, 2-6% of a dispersant, 3-5% of a succinate sulfonate, 1-4% of a disintegrant, 0.1-1% of a binder, 2-12% of a rheological agent, and the balance of a carrier.

[0035] Preferably, the chemical active substance is a combination of difenoconazole and pyraclostrobin, and the mass ratio of the difenoconazole to the pyraclostrobin is (1.8-2.5):(0.6-1), preferably 2:1.

[0036] Preferably, the wetting agent is at least one selected from sodium dodecyl sulfate, calcium dodecylbenzenesulfonate, and alkyl naphthalene sulfonate, and preferably, the wetting agent is sodium dodecyl sulfate.

[0037] Preferably, the dispersant is at least one selected from naphthalene sulfonate formaldehyde condensate, polycarboxylate, and lignin sulfonate, and preferably, the dispersant is naphthalene sulfonate formaldehyde condensate.

[0038] Preferably, the succinate sulfonate is at least one selected from sodium di-iso-octyl succinate sulfonate and sodium di-sec-octyl succinate sulfonate.

[0039] Preferably, the disintegrant is at least one selected from urea, ammonium sulfate, aluminum chloride, and sodium bicarbonate, and preferably, the disintegrant is ammonium sulfate.

[0040] Preferably, the binder is sodium cellulose.

[0041] Preferably, the rheological agent is silicon dioxide.

[0042] Preferably, the carrier is corn starch.

[0043] The fungicide provided by the present application can obviously improve the fungicidal effect of the product by optimizing the formula system by introducing succinate sulfonate and other raw materials, which is reflected in the shortening of the wetting and penetration time of the preparation, the increase of the holding capacity of the liquid medicine and the improvement of the field control effect, so as to achieve the application effect of reducing the amount and increasing the efficiency. The inventor found in the exploration process that by controlling R as C6-C8 alkyl in formula (1), a stable product system can be introduced into the suspension agent, water dispersible granule and emulsion system, which can effectively improve the wetting and penetration effect of the preparation. If the alkyl chain is too long, the improvement of the wetting and penetration effect of the succinate sulfonate on the preparation will decrease, the wetting time will be long, and the subsequent use will be difficult. Further, the inventor found in the exploration process that by controlling the combination of succinate sulfonate, wetting agent and dispersant in the suspension agent system, the wetting time and penetration time of the preparation can be greatly reduced, the wetting is fast, and the maximum stable holding capacity is ≥5μL / cm 2 , which greatly improves the utilization rate of active ingredients. Especially for the suspension agent system of tebuconazole and trifloxystrobin, by simultaneously introducing alkylphenol polyoxyethylene ether phosphate, EO-PO block copolymer and sodium diisooctyl succinate, the wetting time of the product provided is <30s, the penetration time is <130s, and the maximum stable holding capacity is ≥5μL / cm 2 , and the average control effect on corn large spot disease is ≥85%, which is much higher than that of similar products on the market. However, other combinations of wetting agents, dispersants and succinate sulfonates such as triphenylethyl phenol polyoxyethylene ether sulfate, EO-PO block copolymer and sodium diisooctyl succinate cannot guarantee the above comprehensive performance of the preparation at the same time. For the suspension agent system of propiconazole and trifloxystrobin, by simultaneously introducing styrene-anhydride random copolymer, naphthalene sulfonate formaldehyde condensate and sodium di-n-hexyl succinate, the wetting time of the product provided is <30s, the penetration time is <130s, and the maximum stable holding capacity is ≥5μL / cm 2 , and the average control effect on rice sheath blight is ≥80%, which is much higher than that of similar products on the market. However, other combinations of wetting agents, dispersants and succinate sulfonates such as polycarboxylate, naphthalene sulfonate and sodium di-n-hexyl succinate cannot guarantee the above comprehensive performance of the preparation at the same time.

[0044] For boscalid and fludioxonil suspension agent system, by simultaneously introducing fatty alcohol polyoxyethylene ether sulfate, styryl phenol polyoxyethylene polyoxypropylene ether and sodium di-sec-octyl succinate, the wetting time of the product provided is <30s, the penetration time is <130s, and the maximum stable holding capacity is ≥5μL / cm2 , and the average prevention effect on tomato gray mold is ≥70%, which is much higher than that of similar products on the market, while other wetting agents, dispersants, succinate sulfonate combinations such as polyoxyethylene ether potassium phosphate, polycarboxylate, sodium diosecyl succinate cannot guarantee the above-mentioned comprehensive performance of the preparation at the same time.

[0045] For the pyraclostrobin emulsion system, by optimizing the combination of emulsifiers, succinate sulfonates and solvents in the system, especially by simultaneously introducing calcium dodecylbenzenesulfonate, triphenylethyl phenol polyoxyethylene ether and sodium diosecyl succinate under the condition of N,N-dimethyl decanamide as the solvent, the product provided has a wetting time ≤31s, a penetration time <100s and a maximum stable holding volume ≥5μL / cm 2 , and the average prevention effect on water apple brown spot is ≥95%, which is much higher than that of similar products on the market, while other emulsifiers, succinate sulfonate combinations such as dodecylbenzenesulfonic acid ammonium salt and castor oil polyoxyethylene ether cannot guarantee the above-mentioned performance at the same time.

[0046] For the difenoconazole and pyraclostrobin suspension system, by simultaneously introducing triphenylethyl styryl phenol polyoxyethylene ether sulfate ammonium salt, EO-PO block copolymer and sodium diosecyl succinate, the product provided has a wetting time <30s, a penetration time <130s and a maximum stable holding volume ≥5μL / cm 2 , and the average prevention effect on apple brown spot is ≥80%, which is much higher than that of similar products on the market, while other wetting agents, dispersants, succinate sulfonate combinations such as naphthalene sulfonate and anion mixture, EO-PO block copolymer and sodium diosecyl succinate cannot guarantee the above-mentioned comprehensive performance of the preparation at the same time.

[0047] For the difenoconazole water dispersible granule system, by simultaneously introducing sodium dodecyl sulfate, naphthalene sulfonate formaldehyde condensate and sodium diosecyl succinate, the product provided has a wetting time <60s, a penetration time <160s and a maximum stable holding volume ≥5μL / cm 2 , and the average prevention effect on apple brown spot is ≥80%, which is much higher than that of similar products on the market, while other wetting agents, dispersants, succinate sulfonate combinations such as sodium dodecylbenzenesulfonate, polycarboxylate and sodium diosecyl succinate cannot guarantee the above-mentioned comprehensive performance of the preparation at the same time.

[0048] Another aspect of the present application provides a preparation method of a fungicide containing succinate sulfonate, at least comprising the following steps: stirring and mixing the chemical active substance, the succinate sulfonate and the auxiliary agent, then crushing or sand milling, and discharging after detection.

[0049] The third aspect of the present application provides an application of a fungicide containing succinate sulfonate, which is applied to the prevention of fungal diseases of crops. Advantages

[0050] 1. The present application provides a succinate sulfonate-containing fungicide, which improves the utilization rate of fungicidal agricultural active substances by optimizing the fungicide formula system, achieves the purpose of reducing the amount and increasing the effect, and has high market promotion value.

[0051] 2. The fungicide provided by the present application introduces succinate sulfonate into the formula system, cooperates with other raw materials, significantly improves the fungicidal effect of the provided product, shortens the wetting and penetration time of the preparation, increases the holding capacity of the liquid medicine, and improves the field control effect, achieves the application effect of reducing the amount and increasing the effect, and especially controls the alkyl group R in formula (1) to C6-C8, which can be introduced into the suspension agent, water dispersible granule and emulsion system to obtain a stable product system, and effectively improves the wetting and penetration effect of the preparation.

[0052] 3. The present application greatly reduces the wetting time and penetration time of the preparation by controlling the cooperation of succinate sulfonate, wetting agent and dispersant in the suspension agent system, quickly wets, and the maximum stable holding capacity is ≥5 μL / cm 2 , which greatly improves the utilization rate of active ingredients.

[0053] 4. For pyraclostrobin emulsion oil system, by optimizing the cooperation of emulsifier, succinate sulfonate and solvent in the system, especially by simultaneously introducing calcium dodecylbenzenesulfonate, triphenylethyl phenol polyoxyethylene ether, sodium di-n-octyl succinate sulfonate under the condition of N,N-dimethyl decanamide as solvent, the wetting time of the provided product is ≤31 s, the penetration time is <100 s, the maximum stable holding capacity is ≥5 μL / cm 2 , and the average control effect on apple brown spot disease is ≥95%, which is much higher than that of similar products on the market.

[0054] 5. For the difenoconazole water dispersible granule system, by simultaneously introducing sodium dodecyl sulfate, naphthalene sulfonate formaldehyde condensate and sodium di-n-octyl succinate sulfonate, the wetting time of the provided product is <60 s, the penetration time is <160 s, and the maximum stable holding capacity is ≥5 μL / cm 2 , and the average control effect on apple brown spot disease is ≥80%, which is much higher than that of similar products on the market. DETAILED DESCRIPTION

[0055] Example 1

[0056] The succinate sulfonate-containing fungicide provided by the present application comprises the following preparation raw materials in percentage by mass:

[0057] Chemical active substance: 20% tebuconazole, 10% trifloxystrobin;

[0058] Wetting agent: alkylphenol polyoxyethylene ether phosphate 3% (Nanjing Taihua 1101);

[0059] Dispersant: EO-PO block copolymer 2% (Nouryon 500LQ);

[0060] Succinate sulfonate: sodium diisooctyl succinate sulfonate 3%;

[0061] Defoaming agent: SAG1522 0.5%;

[0062] Thixotropic agent: silicon dioxide 1%;

[0063] Thickening agent: xanthan gum 0.2%;

[0064] Antifreeze: propylene glycol 5%;

[0065] Preservative: isothiazolinone 0.1%;

[0066] Deionized water: supplement to 100%.

[0067] Another aspect of the embodiment 1 of the application provides a preparation method of a succinate sulfonate-containing fungicide, comprising the following steps: adding 55.2 grams of deionized water, 20 grams of chemical active substance of tebuconazole with a content of 98wt%, 10 grams of chemical active substance of trifloxystrobin with a content of 98wt%, 3 grams of alkylphenol polyoxyethylene ether phosphate, 2 grams of EO-PO block copolymer, 3 grams of sodium diisooctyl succinate sulfonate, 5 grams of propylene glycol antifreeze, 0.1 gram of isothiazolinone preservative, and 0.5 gram of SAG1522 defoaming agent into a 100mL beaker, and shearing with a shearing homogenizer; in the shearing process, 0.2 grams of xanthan gum and 1 gram of silicon dioxide are added into the beaker, and the shearing is continued until uniform. The sheared uniform sample is poured into a sample pool of an assembled horizontal sand mill for sand milling, and the sample is taken for particle size measurement after sand milling for 10 minutes. When the particle size is less than 3μm, the material is collected, and a 30% tebuconazole trifloxystrobin suspension concentrate is prepared.

[0068] Embodiment 2

[0069] An aspect of the embodiment 2 of the application provides a succinate sulfonate-containing fungicide. The preparation raw materials are as follows in terms of mass percentage:

[0070] Chemical active substance: 25% propiconazole, 10% trifloxystrobin;

[0071] Wetting agent: styrene-anthracene anhydride random copolymer 3% (Croda 550S);

[0072] Dispersant: naphthalene sulfonate formaldehyde condensate 2% (Nanjing Taihua 700#);

[0073] Succinate sulfonate: sodium di-n-hexyl succinate sulfonate 4%;

[0074] Defoaming agent: SAG1522 0.5%;

[0075] Thixotropic agent: magnesium aluminum silicate 1%;

[0076] Thickening agent: xanthan gum 0.1%;

[0077] Antifreeze: propylene glycol 5%;

[0078] Preservative: isothiazolinone 0.1%;

[0079] Deionized water: supplement to 100%.

[0080] The embodiment 2 of the present application provides, in another aspect, a preparation method of a succinate sulfonate-containing fungicide, comprising the following steps: adding 49.3 grams of deionized water, 25 grams of prothioconazole chemical active substance with a content of 98 wt%, 10 grams of trifloxystrobin chemical active substance with a content of 98 wt%, 3 grams of styrene-maleic anhydride random copolymer, 2 grams of naphthalene sulfonate formaldehyde condensate, 4 grams of sodium di-n-hexyl succinate sulfonate, 5 grams of propylene glycol antifreeze, 0.1 gram of isothiazolinone preservative, and 0.5 gram of SAG1522 defoaming agent into a 100 mL beaker, and shearing with a shearing homogenizer; in the shearing process, 0.1 gram of xanthan gum and 1 gram of magnesium aluminum silicate are added into the beaker, and the shearing is continuously performed until uniformity. The sheared uniform sample is poured into a sample cell of an assembled horizontal sand mill for sand milling, and the sand milling is performed for 15 minutes to take a sample for measuring the particle size; when the particle size is less than 4 μm, the material is collected, and a 35% prothioconazole-trifloxystrobin suspension concentrate is prepared.

[0081] Embodiment 3

[0082] The embodiment 3 of the present application provides, in one aspect, a succinate sulfonate-containing fungicide, and the preparation raw materials are as follows in terms of mass percentage:

[0083] Chemical active substance: 25% pyraclostrobin;

[0084] Emulsifier: calcium dodecylbenzenesulfonate 11%;

[0085] Emulsifier: triphenyl ethyl phenol polyoxyethylene ether 9% (Nanjing Taihua 601#);

[0086] Succinate sulfonate: sodium di-n-octyl succinate sulfonate 5%;

[0087] Organic solvent: N,N-dimethyl decanamide, supplement to 100%.

[0088] Embodiment 3 of the present application provides, in another aspect, a method for preparing a succinate sulfonate-containing fungicide, comprising the following steps: adding 50 grams of N,N-dimethyl decanamide, 25 grams of pyraclostrobin chemical active substance with a content of 98 wt% in a 100 mL beaker, starting stirring, and after the chemical active substance is completely dissolved, adding 11 grams of calcium dodecylbenzenesulfonate, 9 grams of triphenylethyl phenol polyoxyethylene ether, and 5 grams of sodium di-n-octyl succinate sulfonate, continuing stirring until clear and transparent, to prepare 250 g / L pyraclostrobin emulsifiable concentrate.

[0089] Embodiment 4

[0090] Embodiment 4 of the present application provides, in one aspect, a succinate sulfonate-containing fungicide, and the preparation raw materials are as follows in terms of mass percentage:

[0091] Chemical active substance: 24% boscalid, 6% fludioxonil;

[0092] Wetting agent: fatty alcohol polyoxyethylene ether sulfate 6% (Zhubenyouqi FS7PG);

[0093] Dispersant: styryl phenol polyoxyethylene polyoxypropylene ether 3% (Nanjing Taihua 33#);

[0094] Succinate sulfonate: di-sec-octyl succinate sodium sulfonate 5%;

[0095] Defoaming agent: SAG1522 0.5%;

[0096] Thixotropic agent: magnesium aluminum silicate 1%;

[0097] Thickening agent: xanthan gum 0.2%;

[0098] Antifreeze: ethylene glycol 5%;

[0099] Preservative: isothiazolinone 0.1%;

[0100] Deionized water: supplement to 100%.

[0101] Embodiment 4 of the present application provides, in another aspect, a method for preparing a succinate sulfonate-containing fungicide, comprising the following steps: adding 49.2 grams of deionized water, 24 grams of boscalid chemical substance with a content of 98 wt%, 6 grams of fludioxonil chemical substance with a content of 98 wt%, 6 grams of fatty alcohol polyoxyethylene ether sulfate, 3 grams of styryl phenol polyoxyethylene polyoxypropylene ether, 5 grams of ethylene glycol antifreeze, 5 grams of succinic acid di-sec-octyl ester sodium sulfonate, 0.1 grams of isothiazolinone preservative, and 0.5 grams of SAG1522 defoaming agent into a 100 mL beaker, shearing with a shear homogenizer, adding 0.2 grams of xanthan gum and 1 gram of magnesium aluminum silicate into the beaker during shearing, and continuing to shear until uniform. Pouring the uniformly sheared sample into a sample cell of an assembled horizontal sand mill for sand milling, sampling after sand milling for 15 minutes, and collecting the sample when the particle size is less than 2 μm, to prepare 30% boscalid fludioxonil suspension concentrate.

[0102] Embodiment 5

[0103] Embodiment 5 of the present application provides, in one aspect, a succinate sulfonate-containing fungicide, the preparation raw materials of which are as follows in terms of mass percentage:

[0104] Chemical active substance: 20% difenoconazole, 10% pyraclostrobin;

[0105] Wetting agent: triphenyl styryl phenol polyoxyethylene ether sulfate ammonium salt 5% (Solvay FD);

[0106] Dispersant: EO-PO block copolymer 6% (BASF PE10500);

[0107] Succinate sulfonate: succinic acid di-2-methyl pentyl ester sodium sulfonate 3%;

[0108] Defoaming agent: SAG1522 0.6%;

[0109] Thixotropic agent: magnesium aluminum silicate 1%;

[0110] Thickening agent: xanthan gum 0.25%;

[0111] Antifreeze: propylene glycol 5%;

[0112] Preservative: isothiazolinone 0.1%;

[0113] Deionized water: supplement to 100%.

[0114] Embodiment 5 of the present application provides, in another aspect, a method for preparing a succinate sulfonate-containing fungicide, comprising the following steps: adding 49.05 grams of deionized water, 20 grams of a chemical active substance of difenoconazole with a content of 98 wt%, 10 grams of a chemical active substance of pyraclostrobin with a content of 98 wt%, 5 grams of triphenyl ethylene phenol polyoxyethylene ether sulfate ammonium salt, 6 grams of an EO-PO block copolymer, 3 grams of sodium di-2-methyl pentyl succinate sulfonate, 5 grams of propylene glycol antifreeze, 0.1 grams of isothiazolinone preservative, and 0.6 grams of SAG1522 antifoaming agent into a 100 mL beaker, shearing with a shearing homogenizer, adding 0.25 grams of xanthan gum and 1 gram of magnesium aluminum silicate into the beaker during shearing, and continuing to shear until uniform. Pouring the sheared and uniform sample into a sample cell of an assembled horizontal sand mill to perform sand milling, sampling after sand milling for 10 minutes, and collecting the sample when the particle size is less than 5 μm, thereby preparing 30% difenoconazole pyraclostrobin suspension concentrate.

[0115] Embodiment 6

[0116] Embodiment 6 of the present application provides, in another aspect, a succinate sulfonate-containing fungicide, the preparation raw materials of which are as follows in terms of mass percentage:

[0117] Chemical active substance: 10% difenoconazole;

[0118] Wetting agent: 2% sodium dodecyl sulfate (Nanjing Guanhua K12);

[0119] Dispersant: 3% naphthalene sulfonate formaldehyde condensate (Jierun Chemical NNO);

[0120] Succinate sulfonate: 5% di-n-octyl sodium succinate sulfonate;

[0121] Rheological agent: 8% silicon dioxide;

[0122] Binder: 0.5% sodium cellulose;

[0123] Disintegrant: 3% ammonium sulfate;

[0124] Carrier: corn starch, supplemented to 100%.

[0125] Embodiment 6 of the present application provides, in another aspect, a method for preparing a succinate sulfonate-containing fungicide, comprising the following steps: uniformly mixing 10 grams of a chemical active substance of difenoconazole with a content of 98 wt%, 2 grams of sodium dodecyl sulfate, 3 grams of naphthalene sulfonate formaldehyde condensate, 0.5 grams of sodium cellulose, 3 grams of ammonium sulfate, 5 grams of sodium dioctyl succinate sulfonate, 8 grams of silicon dioxide, and 68.5 grams of corn starch, crushing the mixture to a fineness of about 8 microns (D90) by using an air flow crusher, adding 12 grams of water to perform kneading granulation, and preparing 10% difenoconazole water dispersible granules when the moisture content is reduced to 3% by drying.

[0126] Comparative Example 1

[0127] Comparative Example 1 of the present application provides a succinate sulfonate-containing fungicide and a method for preparing the same, which has the same specific implementation as Embodiment 1, except that the wetting agent is replaced by triphenylethyl phenol polyoxyethylene ether sulfate (Chubin Oil and Fat FS7PG).

[0128] Comparative Example 2

[0129] Comparative Example 2 of the present application provides a succinate sulfonate-containing fungicide and a method for preparing the same, which has the same specific implementation as Embodiment 2, except that the wetting agent is replaced by polycarboxylate (Ongkhar SCP) and the dispersant is replaced by naphthalene sulfonate (Ongkhar DAC230).

[0130] Comparative Example 3

[0131] Comparative Example 3 of the present application provides a succinate sulfonate-containing fungicide and a method for preparing the same, which has the same specific implementation as Embodiment 3, except that the emulsifier is replaced by dodecyl benzene sulfonic acid ammonium salt 11% (Xinde Chemical DYAY01) and castor oil polyoxyethylene ether 9% (Nanjing Taihua BY110).

[0132] Comparative Example 4

[0133] Comparative Example 4 of the present application provides a succinate sulfonate-containing fungicide and a method for preparing the same, which has the same specific implementation as Embodiment 4, except that the wetting agent is replaced by TSP polyoxyethylene ether potassium phosphate salt (Ongkhar PPS K16) and the dispersant is replaced by polycarboxylate (Wuxi Yijingfeng 7023A).

[0134] Comparative Example 5

[0135] The comparative example 5 of the present application provides a succinate sulfonate-containing fungicide and a preparation method thereof, the specific implementation of which is the same as that of the example 5, except that the wetting agent is replaced by naphthalene sulfonate and anion mixture (Noligen EFW), and the dispersant is replaced by an EO-PO block copolymer (BASF PE10400).

[0136] Comparative example 6

[0137] The comparative example 6 of the present application provides a succinate sulfonate-containing fungicide and a preparation method thereof, the specific implementation of which is the same as that of the example 6, except that the wetting agent is replaced by sodium dodecyl benzene sulfonate (Tiantanrihua LAB), and the dispersant is replaced by polycarboxylate (Debang Chemical HDB-4000).

[0138] Performance test

[0139] 1. The wetting time and penetration time of the formulations provided by the examples and comparative examples are tested by referring to the canvas sinking method GB I1983-1989 immersion method. A specified mass of canvas is placed into a 1000-fold dilution of the formulation, the canvas is wetted and increased in weight by the solution and sinks, the time when the canvas is immersed by the dilution is recorded as the wetting time, and the time when the canvas contacts the liquid surface to sink to the bottom is recorded as the penetration time. The shorter the time, the better the wetting and penetration, which characterize the wetting and penetration of the formulation. The test results are shown in Table 1.

[0140] Table 1

[0141]

[0142] It can be known from the analysis of the test results in Table 1 that the wetting time and penetration time of the formulations provided by the examples 1-6 are shorter than those of the formulations provided by the comparative examples 1-6 and the commercially available products, which indicates that the wetting and penetration effect of the formulations provided by the examples 1-6 is better.

[0143] 2. The holding capacity test, a standard size of plant leaf is cut and weighed (W0, g) by a balance, then held vertically into the dilution of the formulation (diluted by 1000 times) by a pair of tweezers for 4s, the leaf is quickly pulled out of the water surface, and is vertically hung until there is no liquid drop flowing, then weighed (W1, g), the area of the leaf is measured, and the maximum stable holding capacity Rm (μL / cm 2 ) of the leaf is calculated. 2 = (W1-W0) x 1000 / leaf area (cm 2 ), the results are shown in Table 2.

[0144] Table 2

[0145] Maximum stable retention flow rate (μL / cm 2 ) Example 15.36 Example 26.21 Example 37.08 Example 46.11 Example 55.48 Example 65.01 Comparative Example 12.10 Comparative Example 23.12 Comparative Example 33.18 Comparative Example 42.41 Comparative Example 52.16 Comparative Example 62.41 30% tebuconazole + trifloxystrobin SC (commercial product) 1.2535% prothioconazole + trifloxystrobin SC (commercial product) 3.11250 g / L pyraclostrobin EC (commercial product) 3.0130% boscalid + fludioxonil SC (commercial product) 2.5430% difenoconazole + pyraclostrobin SC (commercial product) 2.1410% difenoconazole + pyraclostrobin WG (commercial product) 1.04

[0146] From the analysis of the test results in Table 2, it can be seen that the maximum stable retention flow rate of the formulations provided in Examples 1-6 is higher than that of the formulations provided in Comparative Examples 1-6 and the commercial products.

[0147] 3. Field efficacy test

[0148] (1) The formulation provided in Example 1 was used for the prevention and treatment of corn large spot disease, and the investigation was carried out according to the investigation method of "Guidelines for Pesticide Field Efficacy Test (II) Fungicides for Prevention and Treatment of Corn Large Spot Disease" GB / T 17980.107-2004. Five points were sampled on the diagonal line of each plot, and 5 plants were investigated at each point. The corn large spot disease incidence of all leaves of each plant was investigated.

[0149] Disease classification method: 0 grade: no disease spot; 1 grade: disease spot area accounts for 5% or less of the entire leaf area; 3 grade: disease spot area accounts for 6%-15% of the entire leaf area; 5 grade: disease spot area accounts for 16%-25% of the entire leaf area; 7 grade: disease spot area accounts for 26%-50% of the entire leaf area; 9 grade: disease spot area accounts for 51% or more of the entire leaf area.

[0150] Data statistics: the test data were statistically analyzed by using Duncan's new multiple range method (DMRT) and the test results were evaluated by using Excel and SPSS software.

[0151] [Corrected according to Rule 91 on 18.07.2025] Efficacy calculation method:

[0152] The results are shown in Table 3.

[0153] Table 3

[0154] Average disease index before treatment Average disease index at last investigation Average disease index Average control efficiency (%) Significance of difference Example 10.11 0.68 85.71 a Comparative Example 10.11 1.04 76.72 e 30% tebuconazole + orysastrobin suspension concentrate (commercial product) 0.10 0.82 81.51 bc 75% tebuconazole + orysastrobin water dispersible granule (commercial product) 0.11 0.99 78.93 d 80% tebuconazole wettable powder (commercial product) 0.12 1.04 80.10 cd

[0155] (2) The formulation provided in Example 2 was used for rice sheath blight test, referring to GB / T 17980.20-2000 Pesticide Field Test Guidelines: Fungicides for Controlling Rice Sheath Blight, according to the degree of damage symptoms of rice leaf sheath and leaf, grading, taking each small area as a unit, 5-point sampling method on the diagonal line, investigating 5 clusters connected each point, recording total plant number, diseased plant number and disease level number.

[0156] Disease grading method: 0 level: no disease on the whole plant; 1 level: the fourth leaf and each leaf sheath and leaf below it (with the sword leaf as the first leaf) are diseased; 3 level: the third leaf and each leaf sheath and leaf below it are diseased; 5 level: the second leaf and each leaf sheath and leaf below it are diseased; 7 level: the sword leaf and each leaf sheath and leaf below it are diseased; 9 level: the whole plant is diseased and dies prematurely.

[0157] Data statistics: the test data were statistically analyzed by using Duncan's new multiple range method (DMRT) and the test results were evaluated by using Excel and SPSS software.

[0158] Pharmacodynamic calculation method:

[0159] [Corrected according to Rule 91 on 18.07.2025]

[0160] The test results are shown in Table 4.

[0161] Table 4

[0162] Average disease index before treatment Average disease index at last investigation Average disease index Average control efficiency (%) Significance of difference Example 20.54 3.16 81.65 a A Comparative Example 20.66 4.19 79.40 b AB 35% propiconazole + orysastrobin suspension concentrate (commercial product) 0.62 4.22 78.01 b B 40% propiconazole + tebuconazole suspension concentrate (commercial product) 0.72 5.47 75.37 c C 30% propiconazole dispersible oil suspension concentrate (commercial product) 0.78 6.46 72.82 d D

[0163] (3) The preparation provided in Example 3 is used for apple brown spot disease prevention and treatment, and reference is made to GB / T 17980.124-2004 Pesticide Field Test Guidelines (II) Part 124: Fungicide Prevention and Treatment of Apple Spot Leaf Blight, 40 leaf blades are investigated on each of the east, south, west, north, and middle five parts of each plant, and the number of diseased leaves corresponding to the leaf disease grade is recorded, and 200 leaf blades are investigated in each plot to record the disease grade of each functional leaf.

[0164] Disease leaf grading standard: 0 grade: no disease spot; 1 grade: disease spot area accounts for less than 10% of the entire leaf area; 3 grade: disease spot area accounts for 11%~25% of the entire leaf area; 5 grade: disease spot area accounts for 26%~40% of the entire leaf area; 7 grade: disease spot area accounts for 41%~65% of the entire leaf area; 9 grade: disease spot area accounts for more than 66% of the entire leaf area.

[0165] Data statistics: the test data is statistically analyzed by using Duncan's new multiple range method (DMRT) and evaluated by using Excel and SPSS software.

[0166] [Corrected according to Rule 91 on 18.07.2025] Efficacy calculation method:

[0167] The test results are shown in Table 5.

[0168] Table 5

[0169] Treatment Average disease index before application Last investigation average disease index Average prevention efficiency (%) Significance at 5% Example 3 0.39 0.35 95.17 a Comparative example 3 0.45 2.38 71.65 f 250 g / L pyraclostrobin emulsion (commercial) 0.39 1.38 80.85 e 30% pyraclostrobin suspension concentrate (commercial) 0.40 0.65 91.32 b 25% pyraclostrobin suspension concentrate (commercial) 0.43 1.03 87.32 c 9% pyraclostrobin microcapsule suspension concentrate (commercial) 0.44 1.44 82.16 de

[0170] (4) The preparation provided in Example 4 is used for tomato gray mold disease prevention and treatment, and reference is made to the People's Republic of China National Standard GBT 17980.28-2000 Pesticide Field Test Guidelines (I) Part 28: Fungicide Prevention and Treatment of Vegetable Gray Mold, five random samples are taken in each plot, 2 plants are investigated in each sample, and the following grading method is used for recording.

[0171] Leaf classification method (in leaf units): 0 grade: no lesion; 1 grade: single leaf with 3 lesions; 3 grade: single leaf with 4-6 lesions; 5 grade: single leaf with 7-10 lesions; 7 grade: single leaf with 11-20 lesions, partially dense; 9 grade: single leaf with lesions densely occupying more than one fourth of the leaf area.

[0172] Data statistics: The test data were statistically analyzed by Duncan's new multiple range method (DMRT) using Excel and SPSS software, and the test results were evaluated.

[0173] [Corrected according to Rule 91 on 18.07.2025] Method for calculating efficacy:

[0174] The test results are shown in Table 6

[0175] Table 6

[0176] Treatment Average disease index before application Average control efficiency (%) Significance of difference 5% Example 4 0.367 72.2 a A Comparative Example 4 0.565 57.2 c BC 30% boscalid+fludioxonil suspension concentrate (commercially available) 0.476 64.4 b AB 50% boscalid water dispersible granules (commercially available) 0.387 71.0 a A 50% fludioxonil wettable powder (commercially available) 0.645 51.5 c C

[0177] (5) The formulations provided in Example 5 and Example 6 were used for apple brown spot disease prevention and treatment, and reference was made to GB / T 17980.124-2004 Pesticide Field Efficacy Test Guidelines (II) Part 124 Fungicides for Controlling Apple Spot Leaf Blight, 40 leaves were investigated for each of the five parts of east, south, west, north, and center of each plant, and the number of diseased leaves corresponding to the leaf disease grade was recorded. 200 leaves were investigated in each plot to record the disease grade of each functional leaf.

[0178] Disease leaf classification standard: 0 grade: no lesion; 1 grade: lesion area accounting for less than 10% of the entire leaf area; 3 grade: lesion area accounting for 11%-25% of the entire leaf area; 5 grade: lesion area accounting for 26%-40% of the entire leaf area; 7 grade: lesion area accounting for 41%-65% of the entire leaf area; 9 grade: lesion area accounting for more than 66% of the entire leaf area.

[0179] Data statistics: The test data were statistically analyzed by Duncan's new multiple range method (DMRT) using Excel and SPSS software, and the test results were evaluated.

[0180] [Corrected according to Rule 91 on 18.07.2025] Method for calculating efficacy:

[0181] The results are shown in Table 7.

[0182] Table 7

[0183] Treatment Average diseased leaf rate (%) Average disease index Average control effect (%) Significance at 5% Example 5 15.13 33.44 84.26 a Example 6 18.06 64.05 81.47 b Comparative Example 5 18.13 34.69 78.49 bc Comparative Example 6 24.19 96.24 71.19 cd 30% difenoconazole pyraclostrobin suspension concentrate (commercial product) 21.00 5.21 76.06 cd 10% difenoconazole water dispersible granules (commercial product) 17.50 4.75 77.94 bc

Claims

1. A succinate sulfonate-containing fungicide, characterized by, At least comprising the following components: (a) at least one chemical active substance for preventing and treating fungal diseases of crops, the chemical active substance being selected from one or more of tebuconazole, trifloxystrobin, prothioconazole, cyazofamid, cymoxanil, famoxadone, difenoconazole, pyraclostrobin, boscalid, fludioxonil; (b) at least one succinate sulfonate salt having the structure shown in formula (1): formula (1) wherein R1, R2are both C6-C 12 alkyl; (c) an adjuvant comprising at least one of carriers, disintegrants, binders, rheological agents, dispersants, wetting agents, antifoaming agents, thixotropic agents, antifreezing agents, preservatives, thickening agents, solvents, emulsifiers.

2. The succinate ester sulfonate-containing fungicide according to claim 1, characterized by, The content of the chemical active substance is 10-40% by mass percentage, the content of the succinate sulfonate is 0.5-5%, and the adjuvant makes up the balance.

3. The succinate ester sulfonate-containing fungicide according to claim 1 or 2, characterized in that, In formula (1), R is a C6-C8 alkyl group, preferably any one of the following structures: -(CH 2 )5CH3, -CH2CH (CH3), ( CH2)2CH3, -CH2 CH(C2H5) CH2CH3, -(CH2) 7CH3, -CH(CH3) (CH2)5CH3, -CH2CH(C2H5) (CH2) 3CH3.

4. The succinate ester sulfonate-containing fungicide according to claim 3, characterized by, The formula (1) is obtained by reacting succinic acid and alkyl ester, and the mass percentage of the alkyl ester in the formula (1) is 30-80%.

5. The succinate ester sulfonate-containing fungicide according to claim 3, characterized by, The dosage form of the succinate sulfonate-containing fungicide is one of suspension concentrate, emulsifiable concentrate, granules, wettable powder, and water dispersible granules.

6. The succinate ester sulfonate-containing fungicide according to claim 5, characterized in that, The dosage form of the succinate sulfonate-containing fungicide is suspension concentrate, and the preparation raw materials thereof at least include 20-40% of the chemical active substance, 2-8% of the wetting agent, 2-6% of the dispersant, 3-5% of the succinate sulfonate, 0.1-1% of the antifoaming agent, 0.5-2% of the thixotropic agent, 0.1-0.3% of the thickening agent, 3-6% of the antifreezing agent, 0.05-0.2% of the preservative, and deionized water making up the balance.

7. The succinate ester sulfonate-containing fungicide according to claim 5, characterized in that, The dosage form of the succinate sulfonate-containing fungicide is emulsifiable concentrate, and the preparation raw materials thereof at least include 20-30% of the chemical active substance, 10-30% of the emulsifier, 3-5% of the succinate sulfonate, and organic solvent making up the balance.

8. The succinate ester sulfonate-containing fungicide of claim 5, wherein, The dosage form of the succinate sulfonate-containing fungicide is water dispersible granules, and the preparation raw materials thereof at least include 10-30% of the chemical active substance, 2-6% of the wetting agent, 2-6% of the dispersant, 3-5% of the succinate sulfonate, 1-4% of the disintegrant, 0.1-1% of the binder, 2-12% of the rheological agent, and carrier making up the balance.

9. A process for the preparation of a succino sulfonate-containing fungicide according to any one of claims 1 to 8, characterized in that, At least comprising the following steps: After the chemical active substance, the succinate sulfonate, and the adjuvant are stirred and mixed, they are crushed or sand-milled, and then discharged after passing the detection.

10. Use of a succinate sulfonate-containing fungicide according to any one of claims 1 to 8, characterized in that, Applied to the prevention and treatment of fungal diseases of crops.

Images