CN117882730A - Bi-component weeding composition containing HPPD inhibitor and preparation method thereof - Google Patents

Abstract

The invention discloses a weeding composition containing saflufenacil and an HPPD inhibitor, wherein the weight ratio of the saflufenacil to the HPPD inhibitor in the weeding composition is (100-1): (1-100). The saflufenacil and the HPPD inhibitor act together, have a synergistic effect when in use, reduce the use amount of the weeding composition, achieve good weeding effect, have better compatibility, improve the efficacy stability of the medicine, prolong the storage time of the medicine, avoid demulsification during storage, expand the broad-spectrum weeding effect, have excellent control effects on broadleaf weeds, grassy weeds and sedge weeds, have control effects on resistant weeds, and fill the blank of preventing and killing glyphosate and glufosinate resistant weeds.

Description

Bi-component weeding composition containing HPPD inhibitor and preparation method thereof

Technical Field

The invention relates to a bi-component weeding composition containing an HPPD inhibitor and a preparation method thereof, and relates to A01N, in particular to the field of herbicides.

Background

With the progress of agricultural modernization, the application of herbicide weeding is an important means for improving the agricultural production efficiency, but the application of single-class herbicide weeding easily leads to the occurrence of drug resistance of weeds, reduces the weeding efficiency, and can cause high-dose abuse of the herbicide so as to exacerbate environmental pollution. At present, two or more herbicides are adopted for compounding and use, so that the generation of weed resistance can be obviously reduced, the pesticide consumption is reduced, and the cost is reduced. Therefore, development of a herbicide mixture which can kill resistant weeds, delay the generation of weed resistance, reduce the use amount of pesticides and reduce the environmental influence is important. However, two different pesticide preparations are simply mixed before use, so that incompatibility problems are easy to occur, flocculation and demulsification are caused, the physical stability of the prepared liquid medicine is influenced, and the spray head of a pesticide application device is blocked due to flocculate or sediment, so that the pesticide application effect and efficiency are influenced; the local efficacy is reduced and ineffective due to uneven distribution of the active ingredients in the liquid medicine, and even serious crop injury accidents occur.

Chinese patent No. 202211236697.3 discloses a weeding composition containing saflufenacil and glufosinate-ammonium and application thereof, wherein after the saflufenacil and the glufosinate-ammonium are compounded, the weeding spectrum is enlarged, the weeding effect is improved, the weeding composition has the advantages of quick response, long lasting period, herbicide resistance delay, thorough weeding, low toxicity, safety and environmental protection, but after the application, the cytotoxic agent is accumulated in plants, and a certain pesticide residue possibly exists. The Chinese patent No. 201811225330.5 discloses a weeding composition containing saflufenacil and application thereof, wherein the weeding composition contains A, B two active components, A is saflufenacil, and the two active components are compounded to have obvious synergistic effect, so that the control effect is improved, the pesticide application amount is reduced, but the broad spectrum of weed control is low, and the application range is narrow.

Disclosure of Invention

In order to delay the development of resistance of weeds to herbicides and solve the problem of incompatibility caused by the co-use of two drugs, a first aspect of the present invention provides a two-component herbicidal composition comprising an HPPD inhibitor, which is prepared from the following raw materials, by weight, (100-1): (1-100).

As a preferred embodiment, the weight ratio of saflufenacil to HPPD inhibitor is (50-1): (1-50); preferably, the weight ratio of the saflufenacil to the HPPD inhibitor is (25-1): (1-25); further preferably, the weight ratio of the saflufenacil to the HPPD inhibitor is (10-1): (1-10).

The applicant finds that in the experimental process, a single herbicide is adopted, the weeding range is narrow, and the herbicide resistance of weeds is easy to occur after long-term use, so that the dosage is increased, and the environmental pollution is aggravated. The applicant adopts the synergistic effect of two herbicides of saflufenacil and HPPD inhibitor, and finds good weeding effect, and the possible reasons are hypothesized to be: the target of the saflufenacil is protoporphyrinogen oxidase, and the photosynthesis of plants is blocked by interfering the synthesis of chlorophyll in plant cells so as to achieve the effect of killing weeds; the HPPD inhibitor is targeted to be p-hydroxyphenylpyruvate dioxygenase, the process of converting p-hydroxyphenylpyruvate into homogentisate is blocked by inhibiting the activity of the p-hydroxyphenylpyruvate, so that tocopherol and plastoquinone cannot be normally synthesized, the catalysis of phytoene dehydrogenase (phytoene desaturase, PDS) is blocked, the biosynthesis of carotenoid in the targeted body is further influenced, the albino symptoms of plant meristem and new tissues are promoted, and finally, the plant death is caused, thereby achieving the weeding purpose. The herbicide with two different action mechanisms is mixed, so that the broad spectrum of weeding is enlarged, the occurrence of resistance is delayed, the dosage is reduced, the cost is reduced, and the environmental pollution is lightened.

As a preferred embodiment, the HPPD inhibitor herbicide is selected from one or a combination of several of benzoylpyrazoles, triones and benzoylisoxazoles.

As a preferred embodiment, the benzoylpyrazole herbicide is selected from one of metazodone, amicarbazone, cyclometazachlor, sulfonylgrass pyrazole, pyrazolote, benfurazolidone, (RS) -1- [ 1-ethyl-4- [ 4-methylsulfonyl-3- (2-methoxyethoxy) -o-benzoyl ] -pyrazol-5-oxy ] ethyl carbonate, topramezone, triazolesulfonone, sulfonylgrass pyrazole, fenbuconazole, florasulam, mequindox; the trione herbicide is selected from one of bicyclosultone, dioxopyritrione, fenquinotrione, lancotrione, mesotrione, quinclorac, sulcotrione, fenfluridone, cyclosultone, flupiroxicam and fursultone; the benzoyl isoxazole herbicide is selected from one of clomazone and clomazone.

As a preferred embodiment, the formulation of the herbicidal composition is selected from one of emulsifiable concentrates, microemulsions, aqueous emulsions, dispersible oil suspensions, suspoemulsions, granules, wettable powders, water dispersible granules, microcapsule suspension-suspensions.

As a preferred embodiment, the herbicidal composition is applied to control of non-cultivated weeds; preferably, the herbicidal composition is applied to weed control in industry, business, agricultural construction, public service areas and yards, weed control before crop seeding, fallow and non-crop areas, leisure facilities, pastures before forestation, before crop seeding.

As a preferred embodiment, the herbicidal composition further comprises one or a combination of several of wetting dispersant, emulsifier, thickener, cosolvent, defoamer, preservative, antifreezing agent, water, solvent oil, water-soluble capsule wall material, oil-soluble capsule wall material, stabilizer and carrier.

As a preferred embodiment, the microcapsule suspension-suspension agent is prepared from the following raw materials in parts by weight: 1-10 parts of saflufenacil, 1-20 parts of HPPD inhibitor, 30-50 parts of solvent oil, 1-3 parts of emulsifier, 1-3 parts of oil-soluble capsule wall material, 0.5-1 part of first stabilizer, 0.5-1 part of second stabilizer, 1-5 parts of thickener, 1-5 parts of antifreezing agent, 3-7 parts of wetting dispersant, 0.1-0.5 part of preservative, 0.1-0.5 part of defoamer and water.

As a preferred embodiment, the HPPD inhibitor is a cyclosulfamide.

As a preferred embodiment, the oil-soluble capsule material is isocyanate monomer, and is selected from one or a combination of a plurality of MDI, HMDI, HDI, PAPI.

As a preferred embodiment, the oil-soluble capsule wall material is PAPI (polymethylene polyphenyl polyisocyanate).

As a preferred embodiment, the solvent oil is selected from one or a combination of several of 100#, 150#, and 200# solvent oils. Preferably, the solvent oil is 150# solvent oil.

As a preferred embodiment, the emulsifier is a nonionic surfactant of the alkylphenol series.

As a preferred embodiment, the emulsifier is selected from one or a combination of several of OP-10, NP-9 and OP-7. Preferably, the emulsifier is OP-10 (dodecylphenol polyoxyethylene ether).

The applicant finds that in the experimental process, the microcapsule suspending agent prepared by adopting polymethylene polyphenyl polyisocyanate as an oil-soluble capsule wall material and dodecylphenol polyoxyethylene ether as an emulsifier and 150# solvent oil as an oil phase solvent has remarkable long-acting weeding effect, can obviously prolong weeding aging, and is probably based on the following suspected reasons: the polymethylene polyphenyl polyisocyanate is adopted as an oil-soluble capsule material, the saflufenacil can be wrapped as a core material, the formed core material is not easy to release outwards in a dodecylphenol polyoxyethylene ether system, and the pressure difference between the inner environment and the outer environment of the microcapsule is destroyed by mixing with water during application, so that the saflufenacil is gradually released outwards, a certain release rate is maintained, and the saflufenacil and an HPPD inhibitor outside an oil phase act together, so that the release rate of a medicine is slowed down, the instantaneous loss amount of the medicine after application is reduced, the use time of the herbicide is improved, and the medicine dosage is reduced.

As a preferred embodiment, the thickener is selected from one or a combination of several of xanthan gum, aluminum magnesium silicate, sodium lignin sulfonate, hydroxypropyl cellulose, silica, and polyvinyl alcohol.

As a preferred embodiment, the thickener comprises xanthan gum, sodium lignin sulfonate and polyvinyl alcohol. Preferably, the polyvinyl alcohol is prepared into a polyvinyl alcohol aqueous solution before use, the added mass of the polyvinyl alcohol aqueous solution is 25-35 parts by weight, and the mass concentration of the polyvinyl alcohol aqueous solution is 1-3%.

As a preferred embodiment, the mass ratio of the thickener sodium lignin sulfonate to the xanthan gum is 1: (0.05-0.1). Preferably, the mass ratio of the sodium lignin sulfonate to the xanthan gum is 1:0.075.

as a preferred embodiment, the mass ratio of the thickener to the oil-soluble capsule material is (1-3): 1, preferably, the mass ratio of the thickener to the oil-soluble capsule wall material is (2-3): 1, a step of; preferably, the mass ratio of the thickener to the oil-soluble capsule wall material is 2.15:1.

the applicant finds that in the experimental process, the combination of sodium lignin sulfonate and xanthan gum and the polyvinyl alcohol can form a gel network structure in the oil phase to support the drug microcapsules to prevent the drug microcapsules from settling. When sodium lignin sulfonate and xanthan gum are used as 1: when the weight ratio is (0.05-0.1), the density of the formed oil phase is close to that of the oil-soluble capsule material and the raw material, and the purpose of suspension stability is further realized. Meanwhile, the thickener and the oil-soluble capsule wall material adopt (2-3): the microcapsule suspension system formed by the weight ratio of 1 can maintain a longer suspension state, has good pourability, exceeds the preferred weight ratio range, shortens the suspension stability time, and causes precipitation of a bottom layer of the medicine or poor pourability of the system, and is not easy to flow out and pour during use.

As a preferred embodiment, the first stabilizer is triethanolamine; the second stabilizer is citric acid.

The applicant finds that the prior preparation of the saflufenacil and the HPPD inhibitor is simply mixed in the experimental process, the incompatibility problem can occur between the two single doses, the demulsification and flocculation problems can occur in long-term storage, and the spray dispensing mode is adopted in large-scale agricultural production, so that the spray nozzle is easy to block, and the dispensing efficiency is influenced. In the application, triethanolamine is added into the saflufenacil microcapsule suspension, so that the stability of the drug effect of the saflufenacil is maintained, the structural form of the microcapsule is maintained, a stable emulsion state is formed under the synergistic effect of OP-10, long-term direct contact with cyclosulfamide is avoided, and flocculation problem is avoided. And citric acid with proper weight ratio is added into the suspension of the cyclosulfamide, so that the drug effect of the cyclosulfamide can be kept stable, and the storage time can be prolonged.

As a preferred embodiment, the microcapsule suspension-suspension agent has a particle size of the suspended microcapsules of 1-10 μm.

In a second aspect, the present invention provides a method of preparing a two-component herbicidal composition comprising an HPPD inhibitor, comprising the steps of:

(1) Dissolving saflufenacil, an oil-soluble capsule wall material and an emulsifier in solvent oil to obtain an oil phase, adding a thickener into water to prepare a water phase, adding the oil phase into the water phase under mechanical stirring to form uniform O/W emulsion, adding a first stabilizer into the emulsion, and carrying out polymerization reaction for 1-3 hours at room temperature to obtain the saflufenacil microcapsule; adding an antifreezing agent, supplementing water to 100 parts by weight, and uniformly stirring to obtain the saflufenacil microcapsule suspension;

(2) Adding a wetting dispersant and a second stabilizer into water, stirring and dispersing uniformly, adding an HPPD inhibitor, adding 100 parts by weight in total, shearing uniformly, and then, entering a sand mill for sand milling to obtain an HPPD inhibitor suspending agent;

(3) Mixing the saflufenacil microcapsule suspending agent and the HPPD inhibitor suspending agent, adding the preservative and the defoamer, and mechanically stirring for 1-3 hours to uniformly mix.

Compared with the prior art, the invention has the following beneficial effects:

(1) The bi-component weeding composition containing the HPPD inhibitor has the synergistic effect when in use, and can achieve good weeding effect by reducing the using amount of the weeding composition, the broad-spectrum effect of weeding is increased, and the bi-component weeding composition has good weeding effect on resistant weeds.

(2) The bi-component weeding composition containing the HPPD inhibitor has the advantages that the prepared microcapsule suspending agent has a slow release effect, has long weed removal aging after application, is not easy to volatilize and run off in the environment, reduces the environmental toxicity, and the saflufenacil and the HPPD inhibitor herbicide are reasonably compounded, so that the use dosage can be reduced, the use cost is further reduced, and the environmental pollution is reduced.

(3) The bi-component weeding composition containing the HPPD inhibitor can keep high microcapsule suspension rate, prolong the lasting period, has good pourability and can not cause precipitation problem after long-term storage.

(4) The bi-component weeding composition containing the HPPD inhibitor has good compatibility, can improve the efficacy stability of the drug, prolong the storage time of the drug, avoid demulsification during storage, and avoid blocking a spray head during construction to influence the spraying efficiency.

(5) The bi-component weeding composition containing the HPPD inhibitor expands the broad spectrum of weeding, has excellent control effect on broadleaf weeds, grassy weeds and sedge weeds, has control effect on resistant weeds, and fills the blank of preventing and killing glyphosate and glufosinate resistant weeds.

Detailed Description

Example 1

A bi-component weeding composition containing HPPD inhibitor is prepared into dispersible oil suspending agent, and the preparation raw materials comprise the following components in percentage by mass: 5% of saflufenacil, 10% of HPPD inhibitor, 5% of capramide, 5% of wetting dispersant, 15% of emulsifier, 3% of thickener and 100% of methyl oleate.

The HPPD inhibitor is cyclosulfamide, and the solvent is decyl amide and methyl oleate. The wetting dispersant is purchased from Cantonese agricultural chemical Co., ltd, and has the brand number of HY-8581; the emulsifier is purchased from Daqian high-tech research center limited company and has the brand number of N-600; the thickener is organic bentonite, and is purchased from Suzhou Chinese wood, and the brand is SK-04.

A bi-component weeding composition containing HPPD inhibitor is prepared into dispersible oil suspending agent, and the preparation method comprises the following steps:

(1) The saflufenacil is dissolved in a mixed solvent of the capramide and the methyl oleate, and a wetting dispersant and an emulsifier are added into the solvent and stirred uniformly for standby;

(2) Adding cyclosulfamide to the oil phase under shear;

(3) Grinding under zirconium bead medium to particle size of 2-4 μm.

Example 2

The bi-component weeding composition containing the HPPD inhibitor is prepared into a suspoemulsion, and the preparation raw materials comprise the following components in percentage by mass: 5% of saflufenacil, 5% of HPPD inhibitor, 5% of wetting dispersant, 5% of emulsifier, 20% of cosolvent, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 0.2% of sodium benzoate, 6% of glycol, 0.2% of defoamer and 100% of water.

The HPPD inhibitor is mesotrione, and the wetting dispersant is purchased from Nanjing and has the brand number of 7276-2; the emulsifier is purchased from Nanjing and has the trade marks of 7275-J and 7275-X, and the mass ratio is 9:1, a step of; the cosolvent is a combination of 10wt% cyclohexanone and 10wt% octanamide; the thickener is xanthan gum and aluminum magnesium silicate; the preservative is sodium benzoate; the antifreezing agent is glycol. The defoamer SAG1572, available from Mimex advanced New Material (Nantong) Inc.

A bi-component weeding composition containing an HPPD inhibitor is prepared into a suspending emulsion, and the preparation method comprises the following steps:

(1) Coarse shearing mesotrione, a wetting dispersant and water with the total mass of 1/2, and then putting into a sand mill for sand milling to obtain a suspending agent;

(2) Mixing and heating saflufenacil and cosolvent to 50 ℃ for dissolving and clarifying, adding emulsifier and residual water, and putting into a high-shear emulsifying kettle for shearing to obtain aqueous emulsion;

(3) Mixing a suspending agent and an aqueous emulsion according to a mass ratio of 1:1, adding a thickening agent, a preservative, an antifreezing agent and a defoaming agent, and uniformly stirring and mixing to obtain a finished product.

Example 3

A bi-component weeding composition containing HPPD inhibitor is prepared into granules, and the preparation raw materials comprise the following components in percentage by mass: 1.0% of saflufenacil, 4.0% of HPPD inhibitor, 1% of wetting dispersant, 3% of emulsifier, 1% of capramide, 3% of methyl oleate and 100% of carrier.

The HPPD inhibitor is isoxaflutole; the solvent oil is capramide and methyl oleate; the wetting dispersant is purchased from Cantonese agricultural chemical Co., ltd, and has the brand number of HY-8581; the emulsifier is purchased from Daqian high-tech research center limited company and has the brand number of N-600; the carrier is attapulgite.

A bi-component weeding composition containing HPPD inhibitor is prepared into granules, and the preparation method comprises the following steps:

(1) The method comprises the steps of dissolving saflufenacil in a capramide and methyl oleate solvent, adding a wetting dispersant and an emulsifier into the solution, and uniformly stirring the solution to obtain an oil phase;

(2) Adding isoxaflutole into the oil phase under the shearing action, and grinding under the condition of zirconium bead medium until the grain diameter is 2-4 mu m;

(3) And finally, carrying out carrier adsorption.

Example 4

The bi-component weeding composition containing the HPPD inhibitor is prepared into wettable powder, and the preparation raw materials comprise the following components in percentage by mass: 2% of saflufenacil, 4% of HPPD inhibitor, 5% of solvent oil, 2% of wetting agent, 5% of dispersing agent, 2% of penetrating agent and 100% of carrier.

The HPPD inhibitor is topramezone; the solvent oil is the solvent oil with the number of 150 ℃; the wetting agent is sodium dodecyl benzene sulfonate; the dispersant is purchased from Shanghai high polymer material limited company with the trade name of SD-819; the penetrating agent is azone; the carrier is ammonium sulfate.

A bi-component weeding composition containing an HPPD inhibitor is prepared into wettable powder, and the preparation method comprises the following steps:

(1) The saflufenacil is completely dissolved by solvent oil and then is adsorbed by white carbon black for standby, and then is uniformly mixed with topramezone wetting agent, dispersing agent, penetrating agent and carrier,

(2) Coarsely pulverizing in a mechanical pulverizer, jet pulverizing, and mixing.

Example 5

The bi-component weeding composition containing the HPPD inhibitor is prepared into water dispersible granules, and the preparation raw materials comprise the following components in percentage by mass: 10% of saflufenacil, 20% of HPPD inhibitor, 3% of wetting agent, 8% of dispersing agent, 3% of penetrating agent, 10% of white carbon black, 5% of adhesive and 100% of carrier.

The HPPD inhibitor is mesotrione; the wetting agent is sodium dodecyl benzene sulfonate; the dispersant is purchased from Shanghai high polymer material limited company with the trade name of SD-819; the penetrating agent is azone; the carrier is ammonium sulfate; the binder is polyethylene glycol 6000, which is purchased from Jiangsu province sea-An petrochemical factory.

A bi-component weeding composition containing an HPPD inhibitor is prepared into water dispersible granules, and the preparation method comprises the following steps:

(1) Adding the preparation raw materials into a conical mixer together, uniformly mixing, crushing by an airflow crusher, mixing the crushed materials by the conical mixer, and enabling the fineness of the mixed materials to pass through a 600-mesh standard sieve by 98%;

(2) Adding into a kneader to knead into a plastic material, finally placing the plastic material into an extrusion granulator to extrude and granulate, and drying and sieving the plastic material after granulating.

Example 6

The bi-component weeding composition containing the HPPD inhibitor is prepared into a microcapsule suspension-suspension agent, and the preparation raw materials comprise the following components in parts by weight: 10 parts of saflufenacil, 10 parts of HPPD inhibitor, 40 parts of solvent oil, 3 parts of emulsifier, 1 part of oil-soluble capsule wall material, 0.8 part of first stabilizer, 0.8 part of second stabilizer, 2.75 parts of thickener, 5 parts of antifreezing agent, 5 parts of wetting dispersant, 0.3 part of preservative, 0.3 part of defoamer and water.

The HPPD inhibitor is cyclosulfamide; the solvent oil is 150# solvent oil; the oil-soluble capsule wall material is PAPI; the emulsifier is OP-10; the first stabilizer is triethanolamine; the second stabilizer is citric acid;

the thickener comprises xanthan gum, sodium lignosulfonate and polyvinyl alcohol, wherein the polyvinyl alcohol is prepared into a polyvinyl alcohol aqueous solution before use, the added mass of the polyvinyl alcohol aqueous solution is 30 parts by weight, the mass concentration of the polyvinyl alcohol aqueous solution is 2%, and the mass ratio of the sodium lignosulfonate to the xanthan gum is 1:0.075;

the antifreezing agent is propylene glycol, the wetting dispersant is SP-SC3266, and the antifreezing agent is purchased from Jiangsu qingyu chemical engineering Co.

The preservative is sodium benzoate, the defoamer is an organosilicon defoamer, and the model is SAG1572, which is purchased from a new material of Mai-tui.

A preparation method of a bi-component weeding composition containing an HPPD inhibitor, which is prepared into a microcapsule suspension-suspension agent, comprises the following steps:

(1) Dissolving saflufenacil, an oil-soluble capsule wall material and an emulsifier in solvent oil to be used as an oil phase, adding an oil phase into an aqueous phase by using a polyvinyl alcohol aqueous solution as an aqueous phase under mechanical stirring to form uniform O/W emulsion, adding a first stabilizer into the emulsion, and carrying out polymerization reaction for 1.5 hours at room temperature to obtain a saflufenacil microcapsule; adding sodium lignin sulfonate, xanthan gum, an antifreezing agent and water to 100 parts by weight, and uniformly stirring to obtain the saflufenacil microcapsule suspension;

(2) Adding a wetting dispersant and a second stabilizer into water, stirring and dispersing uniformly, adding an HPPD inhibitor, adding 100 parts by weight in total, shearing uniformly, and then, entering a sand mill for sand milling to obtain an HPPD inhibitor suspending agent;

(3) The saflufenacil microcapsule suspending agent and the HPPD inhibitor suspending agent are mixed according to the mass ratio of 1:1, adding preservative sodium benzoate and defoamer SAG1572, and mechanically stirring for 2 hours to uniformly mix.

Comparative example 1

A bi-component weeding composition containing HPPD inhibitor is prepared into microcapsule suspension-suspension agent, and the preparation raw materials and the preparation method are the same as in example 6, except that the dispersing agent is sodium lignin sulfonate.

Comparative example 2

A bi-component herbicidal composition containing HPPD inhibitor is prepared as a microcapsule suspension-suspension agent, which is prepared as a raw material and a preparation method as in example 6 except that the solvent is cyclohexanone.

Comparative example 3

A two-component herbicidal composition containing an HPPD inhibitor was prepared as a microcapsule suspension-suspension agent, which was prepared as a starting material and a preparation method as in example 6 except that the second stabilizer was sodium citrate.

Comparative example 4

A two-component herbicidal composition containing an HPPD inhibitor was prepared as a microcapsule suspension-suspension agent, which was prepared as a raw material and a preparation method as in example 6 except that the thickener was 3.00 parts.

Performance test:

1. stability:

(1) Thermal storage stability

About 30mL of the sample was injected into a clean ampoule with a syringe, and sealed with an alcohol burner. At least 3 bottles were sealed and weighed separately. Placing the sealed ampoule bottle in a constant temperature box with the temperature of (54+/-2), placing for 14d, taking out, wiping the outside of the ampoule bottle, weighing the ampoule bottle, and testing a specified item within 24h after the ampoule bottle is wiped clean.

(2) Low temperature stability

The 50mL sample was placed in a 100mL beaker and cooled to (0.+ -. 1) C by appropriate means and held for 1h, during which time it was stirred with a glass rod, and no solids or oil precipitated to be acceptable.

(3) Suspension rate

Preparing 1wt% suspension with standard water, standing in a specified measuring cylinder at constant temperature for 45min, taking out the upper layer 9/10 suspension, measuring the content of effective components in the bottom 1/10 suspension, and calculating the content of effective components in the upper layer 9/10 suspension.

(4) Pourability of

According to standard GB/T31737.

The test results are shown in Table 1.

TABLE 1

2. The results of the determination of the toxicity of the bupirimate and the cyclosulfamide and the compound thereof to weeds are shown in Table 2.

Test purpose: the control effect of the saflufenacil, the cyclosulfamone and different mixed combinations thereof on barnyard grass and dayflower is measured under the condition of greenhouse potting, and the combined effect of the mixed use is evaluated.

The test method comprises the following steps: potted plant test, barnyard grass and dayflower are used as target weeds. Test methods refer to "NY/T1155.1-2006-pesticide indoor bioassay test guidelines-herbicide-part 3-activity assay-stem and leaf spray method". The size of the plastic culture basin is as follows: the diameter of the lower opening is 18.5, the diameter of the upper opening is 27cm, and the height is 15cm. The soil without herbicide (pH value 6.8, organic matter content 2.5%) was uniformly sown with 30 seeds per pot, the stem and leaf spraying treatment was carried out with spray towers at 3-4 leaf stages of weeds, each treatment was repeated 3 times, and a blank control was set. And observing and investigating the number of surviving weed strains 21d after the drug, and calculating the plant prevention effect. The combined effect of the blends was evaluated using the Gowing method.

Theoretical prevention effect

In the above formula:

x is the weed control effect when the quantity of the saflufenacil is A;

y is weed control effect when the dosage of the cyclosulfamide is B;

E ₀ the herbicide has theoretical prevention effect when the herbicide saflufenacil is mixed with the herbicide A+cyclosulfamide B;

e is the actual measurement control effect of the mixed herbicide of which the quantity of the saflufenacil is A and the quantity of the cyclosulfamide is B;

when E-E0 is more than 10, the synergistic effect is achieved; when E-E0 is less than or equal to-10 and less than or equal to-10, the addition effect is achieved; when E-E0 < -10, antagonism is provided.

TABLE 2

The bupirimate and the HPPD inhibitor cyclosulfamone are mixed to show obvious synergistic effect; when the saflufenacil and the cyclosulfamone are mixed when the dosage is high, the weeding effect reaches 100 percent, and E-E0 is less than or equal to 10, which shows additive effect.

3. Field efficacy test

(1) Test materials

(1) Test crop and test subject: selecting non-cultivated land with barnyard grass, green bristlegrass, dayflower and abutilon

(2) Test agent: 3 saflufenacil+cyclosulfamone compound preparation products with different proportions

(3) Contrast agent: 30% glyphosate isopropylamine salt aqueous solution, 10% refined glufosinate solution, 33%2 methyl glyphosate aqueous solution, 32% saflu glyphosate dispersible oil suspending agent

(2) Test instrument:

sprayer, bucket, pipette, graduated flask, beaker, level, etc.

(3) Test content and method

According to the dosage requirements of the test medicament and the control medicament, dividing test cells, wherein each cell is provided with a 50cm isolation zone, and the test cells are arranged in random groups.

The knapsack sprayer is adopted, and the application weather is carried out when the choice is clear, so that the condition that the rainwater is not met 24 hours after the medicine is applied is ensured.

The weed population in the plot is recorded by an estimation method, and the symptoms (such as production inhibition, green loss, deformity and the like) causing weed injury after the application are described in detail, and the final plant prevention effect is comprehensively estimated.

(4) Test results

The test results are shown in Table 3.

TABLE 3 Table 3

The bupirimate and the cyclosulfamide are mixed for use, and the comprehensive weeding effect on grassy barnyard grass, green bristlegrass, dayflower and abutilon is better than that of 30% glyphosate isopropylamine salt aqueous solution, 10% refined glufosinate solution, 32%2 methyl glyphosate aqueous solution and 32% saflu glyphosate dispersible oil suspending agent; the weeding spectrum of the bupirimate mixed with the cyclosulfamide is wider.

Claims (10)

1. The bi-component weeding composition containing the HPPD inhibitor is characterized in that the preparation raw materials comprise saflufenacil and the HPPD inhibitor, wherein the weight ratio of the saflufenacil to the HPPD inhibitor is (100-1): (1-100).

2. The two-component herbicidal composition containing an HPPD inhibitor according to claim 1, wherein the HPPD inhibitor is selected from one or a combination of several of benzoyl pyrazole herbicides, triones herbicides, benzoyl isoxazole herbicides.

3. The two-component herbicidal composition containing an HPPD inhibitor according to claim 2, wherein the benzoylpyrazole herbicide is selected from one of metazachlor, amicarbazone, ciclopirox, sulfonyloxazomet, topiramate, clomazone, (RS) -1- [ 1-ethyl-4- [ 4-methylsulfonyl-3- (2-methoxyethoxy) -o-benzoyl ] -pyrazol-5-oxy ] ethylcarbonate, topramezone, triazolesulfone, sulfonyloxazomet, benzofluorfen, fluorsulfone oxamate, mequindox; the trione herbicide is selected from one of bicyclosultone, dioxopyritrione, fenquinotrione, lancotrione, mesotrione, quinclorac, sulcotrione, fenfluridone, cyclosultone, flupiroxicam and fursultone; the benzoyl isoxazole herbicide is selected from one of clomazone and clomazone.

4. The two-component herbicidal composition comprising an HPPD inhibitor according to claim 1, wherein the formulation of the herbicidal composition is selected from one of emulsifiable concentrates, microemulsions, aqueous emulsions, dispersible oil suspensions, suspoemulsions, granules, wettable powders, water dispersible granules, microcapsule suspension-suspensions.

5. The two-component herbicidal composition comprising an HPPD inhibitor according to claim 4, further comprising one or more of a wetting dispersant, an emulsifier, a thickener, a cosolvent, a defoamer, a preservative, an antifreezing agent, water, a solvent oil, a water-soluble capsule, an oil-soluble capsule, a stabilizer, and a carrier.

6. The two-component herbicidal composition containing an HPPD inhibitor according to claim 5, wherein the formulation of the herbicidal composition is a microcapsule suspension-suspension agent comprising, in parts by weight: 1-10 parts of saflufenacil, 1-20 parts of HPPD inhibitor, 30-50 parts of solvent oil, 1-3 parts of emulsifier, 1-5 parts of oil-soluble capsule wall material, 0.5-1 part of first stabilizer, 0.5-1 part of second stabilizer, 1-2 parts of thickener, 1-5 parts of antifreezing agent, 3-7 parts of wetting dispersant, 0.1-0.5 part of preservative, 0.1-0.5 part of defoamer and water.

7. The two-component herbicidal composition comprising an HPPD inhibitor according to claim 6, wherein the oil-soluble capsule wall material is an isocyanate monomer selected from one or a combination of several of MDI, HMDI, HDI, PAPI.

8. The two-component herbicidal composition comprising an HPPD inhibitor according to claim 6, wherein the thickener is selected from one or more of xanthan gum, magnesium aluminum silicate, sodium lignin sulfonate, hydroxypropyl cellulose, silica, polyvinyl alcohol.

9. The two-component herbicidal composition comprising an HPPD inhibitor according to claim 6, wherein the suspended microcapsules in the microcapsule suspension-suspension agent have a particle size of 1 to 10 μm.

10. A process for the preparation of a two-component herbicidal composition comprising an HPPD inhibitor according to any one of claims 6 to 9, characterized by comprising the steps of:

(1) Dissolving saflufenacil, an oil-soluble capsule wall material and an emulsifier in solvent oil to obtain an oil phase, adding a thickener into water to prepare a water phase, adding the oil phase into the water phase under mechanical stirring to form uniform O/W emulsion, adding a first stabilizer into the emulsion, and carrying out polymerization reaction for 1-3 hours at room temperature to obtain the saflufenacil microcapsule; adding an antifreezing agent, supplementing water to 100 parts by weight, and uniformly stirring to obtain the saflufenacil microcapsule suspension;

(2) Adding a wetting dispersant and a second stabilizer into water, stirring and dispersing uniformly, adding an HPPD inhibitor, adding 100 parts by weight in total, shearing uniformly, and then, entering a sand mill for sand milling to obtain an HPPD inhibitor suspending agent;

(3) Mixing the saflufenacil microcapsule suspending agent and the HPPD inhibitor suspending agent, adding the preservative and the defoamer, and mechanically stirring for 1-3 hours to uniformly mix.