Pesticide preparation containing mesotrione-ametryn-triclopyr and preparation method thereof
By combining herbicides such as nitrosulone, amarin and triclopido and other additives, a high-utility pesticide preparation was prepared, which solved the problems of low utilization rate and weed resistance of existing herbicides and achieved more effective herbicide effects.
Patent Information
- Application Number
- CN202411756983.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-03
- Publication Date
- 2025-03-07
AI Technical Summary
Existing herbicides are less utilizing in sugarcane planting environments, and the use of the same herbicide for a long time can easily lead to weed resistance.
A pesticide preparation containing nitrosulone-amemencen-triclopyridium and its preparation method are used to prepare pesticide preparations with high utilization rates by combining these herbicides and other additives.
Improves the utilization rate of herbicides, reduces the risk of weed resistance, and achieves better herbicide effects.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of pesticides, and in particular to a pesticide preparation containing mesotrione-ametryn-triclopyr and a preparation method thereof. Background Art
[0002] Sugar is one of my country's important agricultural products and is related to social stability and development. As the basic raw material for sugar, the development of the sugar industry is crucial to ensuring the security of sugar supply. In the 2020 / 2021 crushing season, my country's sugarcane sugar production accounted for 85.6% of the total sugar production. As an important raw material crop for sugar, sugarcane will be invaded by a variety of diseases, insects and weeds during the planting process, which seriously affects the yield and sugar content of sugarcane. Chemical control is still the main means of preventing and controlling sugarcane diseases, insects and weeds, and plays an irreplaceable role in ensuring the safety of sugarcane production.
[0003] During the planting process of sugarcane, there are many types of weeds in the sugarcane field, and the weeds in the field vary greatly. They will compete with the sugarcane for water and nutrients, and have a great impact on the quality and yield of the sugarcane. In the field where weeds are seriously harmful, the sugarcane yield can be reduced by 30%-70%. At present, chemical control is the main method for weed control in sugarcane production. The most commonly used herbicides are mesotrione, ametryn, triclopyr butoxyethyl, atrazine, diuron, etc. These herbicides have a good effect on annual weeds in sugarcane fields. Mesotrione and butoxyethyl triclopyrazone are herbicides that are para-hydroxyphenylpyruvate dioxidase (HPPD) inhibitors. HPPD is necessary for the growth of weeds and is involved in the biosynthesis of plastoquinone and tocopherol in plants. These two substances play a key role in the photosynthesis and antioxidant processes of plants. By inhibiting HPPD, these biosynthesis pathways in plants can be blocked, resulting in the inability of plants to photosynthesize normally, ultimately leading to plant death. Amethoxazole is a selective systemic herbicide and a typical photosynthesis inhibitor. It is absorbed by the leaves, stems or roots of weeds and conducted in the plant body, thereby affecting the normal physiological functions of the plant and ultimately leading to the death of the weeds.
[0004] Herbicides are usually prepared into wettable powders or suspensions, but a single herbicide has a small weed control spectrum, weed damage cannot be effectively suppressed and reduced, and it is often difficult to control their spread and growth. In addition, long-term use of the same herbicide can easily cause weeds to develop resistance. Therefore, composite herbicides are currently used more frequently. For example, patent technical document CN103798252B discloses a mesotrione composite herbicide. The composite herbicide in the invention contains three active ingredients: mesotrione, bentazone, and bispyribac-butyl, wherein the weight ratio of mesotrione, bentazone, and bispyribac-butyl is 1-30:1-30:1-20. By using a composite of several herbicides, a broad-spectrum weed control effect can be achieved. However, sugarcane is planted in a high temperature and high humidity environment, which has a great impact on the utilization rate of the herbicide, that is, the utilization rate of the herbicide needs to be improved.
[0005] Therefore, according to the above-mentioned related technologies, it is urgent to develop a pesticide preparation containing mesotrione-ametryn-triclopyr and a preparation method thereof. Summary of the invention
[0006] In view of this, the object of the present invention is to provide a pesticide formulation containing mesotrione-ametryn-triclopyr and a preparation method thereof, so as to solve the problem of poor utilization rate of herbicides in the prior art.
[0007] Based on the above purpose, the present invention provides a pesticide preparation containing mesotrione-ametryn-triclopyr and a preparation method thereof.
[0008] A pesticide preparation containing mesotrione-ametryn-triclopyr, prepared from the following raw materials in parts by weight:
[0009] 3-6 parts of mesotrione, 27.5-55 parts of ametryn, 5-10 parts of butoxyethyl triclopyr, 32-42 parts of emulsifier, 3-5 parts of wetting agent, 3-5 parts of dispersant, 0.3-0.8 parts of thickener, 0.4-0.7 parts of antifreeze agent, 0.1-0.3 parts of organosilicon defoamer, 0.5-1 parts of preservative, 3.4-5.2 parts of auxiliary agent, 10-13 parts of deionized water;
[0010] The auxiliary agent is obtained by mixing auxiliary agent A and auxiliary agent B in a mass ratio of 27-33:8-14;
[0011] The auxiliary agent A is obtained by mixing composite nanoparticles and methyl oleate auxiliary agent in a mass ratio of 3-7:1.8-4.5;
[0012] The auxiliary agent B is prepared from biochar, composite nanoparticles and Deinococcus agent;
[0013] The mass ratio of the biochar, the composite nanoparticles and the Deinococcus agent is 8-12:3.3-4.5:15.5-18.7;
[0014] The composite nanoparticles are obtained by mixing tannin powder and modified lignin in a mass ratio of 0.8-1.3:2-2.5.
[0015] Preferably, the preparation method of the modified lignin is as follows:
[0016] Step A1. Add wood powder, deionized water and acetone into an autoclave reactor, heat and reflux at 185-200°C for 110-130 min, extract with dichloromethane at 30-40°C for 30-40 min, and then collect the obtained extract by rotary evaporation and dry to obtain lignin powder;
[0017] Step A2. Place lignin powder and dimethyl sulfate in a flask, heat and reflux at 72-78° C. for 130-150 min, add a 2 mol / L hydrochloric acid solution, and then wash twice with deionized water to obtain a mixture A;
[0018] Step A3. The mixture A, diglycidyl ether and N,N-dimethylbenzylamine are heated to reflux, filtered, washed with a mixture of petroleum ether and deionized water, and dried at 50-60° C. for 48-55 hours to obtain modified lignin.
[0019] Preferably, the ratio of wood powder, deionized water and acetone in step A1 is 2-3 g: 12-15 mL: 30-36 mL;
[0020] The ratio of lignin to dimethyl sulfate and hydrochloric acid solution in step A2 is 1 mol: 2.4-2.7 mol: 8-13 mL;
[0021] In step A3, the molar ratio of the mixture A to diglycidyl ether and N,N-dimethylbenzylamine is 1:0.4-0.6:0.02-0.05;
[0022] The volume ratio of petroleum ether to deionized water in the petroleum ether-deionized water mixture is 1:1-1.2;
[0023] The temperature during the heating reflux is 90-100° C. and the time is 5-6 hours.
[0024] Preferably, the preparation method of the auxiliary agent A is as follows:
[0025] Step B1. Add bark powder, deionized water and acetone into a three-necked flask, heat and reflux at 45-50° C. for 90-120 min to obtain a tannin-rich liquid, remove the acetone by evaporation, add deionized water to precipitate insoluble tannin, and then centrifuge and freeze-dry to obtain tannin powder;
[0026] Step B2. The modified lignin, tannin powder, deionized water and acetone were placed in an ultrasonic bath and mixed evenly, and then 25-28 mL of deionized water was added using a constant flow pump, and the composite nanoparticles were collected by centrifugation and freeze drying;
[0027] Step B3. adding the composite nanoparticles to the ethyl oleate additive and mixing them evenly to obtain additive A;
[0028] The ratio of the bark powder, deionized water and acetone in step B1 is 4-5 g: 12-15 mL: 30-38 mL;
[0029] The usage ratio of the modified lignin, tannin powder, deionized water and acetone in step B2 is 0.8-1.3 g: 2-2.5 g: 15-18 mL: 35-40 mL.
[0030] Preferably, the preparation method of the auxiliary agent B is as follows:
[0031] Step C1. After washing, crushing and drying the sugarcane straw, carbonizing it at 450-500°C, taking 5g of it and soaking it in 20-25g of a 40% KOH solution by mass, stirring it for 12-13h, letting it stand for 20-24h, drying it at 110-120°C for 48-50h, cooling it, washing it twice with a 1mol / L hydrochloric acid solution and deionized water, and then drying it at 60-70°C for 3-4h to obtain biochar;
[0032] Step C2. Inoculate the surface of TGY solid culture medium with Deinococcus by coating method, and culture at 30°C for 48-72h, then inoculate in TGY liquid culture medium, culture at 30°C for 24-48h at a speed of 180-200rpm, and finally centrifuge at 4000-5000rpm for 15-20min, discard the supernatant, collect the bacteria, and prepare a bacterial suspension with sterile water to obtain Deinococcus agent;
[0033] Step C3. Add biochar and composite nanoparticles to the Deinococcus agent, and place the conical flask in a constant temperature shaking incubator set at a temperature of 28-32°C and a rotation speed of 130-160 r / min for 20-24 hours, take it out and let it stand for 2-3 hours, filter it, rinse it with sterile water, and filter it to obtain additive B;
[0034] The TGY solid culture medium in step C2 is formulated as follows: 0.5% tryptone, 0.3% yeast extract, 0.1% glucose, 1.5% agar, and a pH of 7.0-7.2;
[0035] The formula of the TGY liquid culture medium is: 0.5% tryptone, 0.3% yeast extract, 0.1% glucose, and pH is 7.0-7.2.
[0036] Preferably, the emulsifier is emulsifier 72-F;
[0037] The wetting agent is any one of sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, and sodium lauryl sulfate;
[0038] The dispersant is a modified lignin sulfonate;
[0039] The thickener is any one of xanthan gum, magnesium aluminum silicate, polyvinyl alcohol and organic bentonite;
[0040] The antifreeze agent is any one of ethylene glycol, glycerol, polyethylene glycol and urea;
[0041] The preservative is Kathon.
[0042] Preferably, the preparation method of the modified lignin sulfonate is as follows:
[0043] Step D1. The alkali lignin and a 10% sodium hydroxide aqueous solution are uniformly stirred, the temperature is raised to 70-75°C, formaldehyde is added dropwise, and the temperature is kept for 1.5-2h, the temperature is raised to 92-97°C again, anhydrous sodium sulfite is added, and the temperature is kept for 2-2.5h, and the mixture is washed twice with anhydrous ethanol, dialyzed, concentrated by rotary evaporation, and freeze-dried to obtain sulfomethylated lignin;
[0044] Step D2. After dissolving the sulfomethylated lignin in water, add sodium hydroxide to adjust the pH value to 11, increase the system temperature to 78-83°C, add potassium iodide and 1,6-dibromohexane, wash twice with anhydrous ethanol after 4.5-5.5 hours, dialyze, concentrate by rotary evaporation, and freeze-dry to obtain modified lignin sulfonate.
[0045] Preferably, the mass ratio of alkali lignin, sodium hydroxide aqueous solution, formaldehyde and anhydrous sodium sulfite in step D1 is 9.5-11:13-15:1:5.3-6;
[0046] The mass ratio of the sulfomethylated lignin, potassium iodide and 1,6-dibromohexane in step D2 is 10-12:0.1-0.2:0.8-1.5.
[0047] A method for preparing a pesticide preparation containing mesotrione-ametryn-triclopyr, comprising the following steps:
[0048] Step S1. After deionized water, dispersant, wetting agent, silicone defoamer and antifreeze are mixed evenly, ametryn is added, and the mixture is sheared for the first time. The mixture is then poured into a sand mill containing zirconium beads and sand milled for 1.5-2.0 hours. After the particle size is sand milled to less than 0.5 μm, the liquid medicine is filtered out to obtain a mixture B.
[0049] Step S2. After mesotrione, butoxyethyl triclopyr and an emulsifier are uniformly mixed, mixture B is added, and a second shearing is performed. After a thickener, a preservative and an adjuvant are added, a third shearing is performed to obtain a pesticide preparation containing mesotrione-ametryn-triclopyr.
[0050] Preferably, the speed of the first shearing in step S1 is 5000-6000 r / min, and the time is 10-15 min;
[0051] The speed of the second shearing in step S2 is 3000-3500 r / min, and the time is 12-17 min;
[0052] The speed of the third shearing in step S2 is 4500-5000 r / min, and the time is 8-13 min.
[0053] Beneficial effects of the present invention:
[0054] The invention provides a pesticide preparation containing mesotrione-ametryn-triclopyr and a preparation method thereof. The invention prepares a pesticide preparation with high utilization rate by compounding three herbicides, namely mesotrione, butoxyethyl triclopyr and ametryn, with other additives.
[0055] Among them, the adjuvants in other additives are composed of adjuvant A and adjuvant B. Adjuvant A is obtained by mixing composite nanoparticles with methyl oleate adjuvant. The composite nanoparticles can have good biocompatibility in pesticide preparations, and work together with methyl oleate adjuvant and modified lignin sulfonate dispersant to have good wettability, so that the herbicide can be evenly spread on the leaf surface, thereby improving the utilization rate; adjuvant B is prepared from biochar, composite nanoparticles and Deinococcus agent, and can adsorb the herbicide and reduce the leaching and migration of the original drug while having an ultraviolet shielding effect. Through the combined use of adjuvant A and adjuvant B, the maximum utilization of the herbicide is achieved. Compared with the existing technology, it has broad application prospects. DETAILED DESCRIPTION
[0056] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.
[0057] The sources and properties of some of the raw materials used in the present invention are as follows:
[0058] Bark powder was purchased from Xi'an Shangcheng Biotechnology Co., Ltd.; acetone was purchased from Lihua Yiweiyuan Chemical Co., Ltd.; wood powder was purchased from Pingyi County Lingfeng Wood Powder Co., Ltd.; dichloromethane was purchased from Shandong Hailong Chemical Co., Ltd.; dimethyl sulfate was purchased from Xinjiang Jinshenghui Chemical Co., Ltd.; diglycidyl ether was purchased from Nantong Runfeng Petrochemical Co., Ltd.; N,N-dimethylbenzylamine was purchased from Wuhan Kemik Biomedical Technology Co., Ltd.; emulsifier 72-F was purchased from Wuhan Adama New Energy Co., Ltd.; sodium dodecyl sulfate was purchased from Guangzhou Dingguo Biotechnology Co., Ltd.; xanthan gum was purchased from Shandong Aicai Biotechnology Co., Ltd.; urea was purchased from Anhui Jinmei Zhongneng Chemical; Kason was purchased from Kason Technology Co., Ltd.;
[0059] The Deinococcus used in the present invention is Deinococcus radiodurans RUV-113CGMCC No. 2960, which is disclosed in the invention patent with the authorization announcement number of "CN101591630B" and the name of "A kind of Deinococcus radiodurans and the microbial anti-ultraviolet radiation preparation produced therefrom", and the deposit number is CGMCC No. 2960.
[0060] Example 1: A method for preparing a pesticide preparation containing mesotrione-ametryn-triclopyr, comprising the following steps:
[0061] S1. 2 g of wood powder, 12 mL of deionized water and 3 mL of acetone were added to an autoclave reactor, heated under reflux at 185 ° C for 110 min, extracted with dichloromethane at 30 ° C for 30 min, and then the obtained extract was collected by rotary evaporation and dried to obtain lignin powder;
[0062] S2. 1 mol of lignin powder and 2.4 mol of dimethyl sulfate were placed in a flask, heated under reflux at 72°C for 130 min, and then 8 mL of 2 mol / L hydrochloric acid solution was added, followed by washing twice with deionized water to obtain a mixture A;
[0063] S3. 1 mol of mixture A, 0.4 mol of diglycidyl ether and 0.02 mol of N,N-dimethylbenzylamine were heated to reflux at 90°C for 5 h, filtered, washed with a mixture of petroleum ether and deionized water in a volume ratio of 1:1, and dried at 50°C for 48 h to obtain modified lignin;
[0064] S4. 4 g of bark powder, 12 mL of deionized water and 30 mL of acetone were added to a three-necked flask, heated and refluxed at 45° C. for 90 min to obtain a tannin-rich liquid, the acetone was removed by evaporation, deionized water was added to precipitate insoluble tannins, and then centrifuged and freeze-dried to obtain tannin powder;
[0065] S5. 0.8 g of modified lignin, 2 g of tannin powder, 15 mL of deionized water and 35 mL of acetone were placed in an ultrasonic bath and mixed evenly, and then 25 mL of deionized water was added using a constant flow pump, and the composite nanoparticles were collected by centrifugation and freeze drying;
[0066] S6. Add 3 g of the composite nanoparticles to 1.8 g of ethyl oleate additive and mix well to obtain additive A;
[0067] S7. After washing, crushing and drying the sugarcane straw, carbonizing it at 450°C, taking 5g of it and soaking it in 20g of a 40% KOH solution, stirring it for 12h, letting it stand for 20-24h, drying it at 110°C for 48h, cooling it, washing it twice with a 1mol / L hydrochloric acid solution and deionized water, and then drying it at 60°C for 3h to obtain biochar;
[0068] S8. Inoculate the surface of TGY solid culture medium with Deinococcus by coating method, and culture at 30°C for 48h, then inoculate in TGY liquid culture medium, culture at 30°C for 24h at a speed of 180rpm, and finally centrifuge at 4000rpm for 15min, discard the supernatant, collect the bacteria, and prepare a bacterial suspension with sterile water to obtain Deinococcus agent;
[0069] S9. Add 8 g of biochar and 3.3 g of composite nanoparticles to 15.5 g of the Deinococcus agent, and place the conical flask in a constant temperature shaking incubator set at 28° C. and 130 r / min for 20 h, take it out and let it stand for 2 h, filter it, rinse it with sterile water, and filter it to obtain additive B;
[0070] S10. 9.5 g of alkali lignin and 13 g of a 10% sodium hydroxide aqueous solution were stirred evenly, and 1 g of formaldehyde was added dropwise after the temperature was raised to 70 ° C. The mixture was kept warm for 1.5 h, and 5.3 g of anhydrous sodium sulfite was added after the temperature was raised to 92 ° C. The mixture was kept warm for 2 h, and the mixture was washed twice with anhydrous ethanol, dialyzed, concentrated by rotary evaporation, and freeze-dried to obtain sulfomethylated lignin;
[0071] S11. After 10 g of sulfomethylated lignin was dissolved in water, sodium hydroxide was added to adjust the pH value to 11, the system temperature was raised to 78 ° C, 0.1 g of potassium iodide and 0.8 g of 1,6-dibromohexane were added, and after 4.5 h, it was washed twice with anhydrous ethanol, dialyzed, concentrated by rotary evaporation, and freeze-dried to obtain modified lignin sulfonate;
[0072] S12. 10 g of deionized water, 3 g of modified sodium lignin sulfonate, 3 g of sodium dodecyl sulfate, 0.1 g of silicone defoamer, and 0.4 g of urea were mixed and then 27.5 g of amethoxazole was added. The mixture was sheared for the first time at a speed of 5000 r / min for 10 min, and then poured into a sand mill containing zirconium beads and sanded for 1.5 h. After the particle size was sanded to less than 0.5 μm, the liquid was filtered out to obtain a mixture B;
[0073] S13. After uniformly mixing 3g of mesotrione, 5g of butoxyethyl triclopyr and 32g of emulsifier 72-F, add mixture B, and perform a second shearing at a speed of 3000r / min for 12min. Then, add 0.3xanthan gum, 0.5g of kason and 3.4g of auxiliary agent, and perform a third shearing at a speed of 4500r / min for 8min. The mass ratio of auxiliary agent A to auxiliary agent B in the auxiliary agent is 27:8, so as to obtain a pesticide preparation containing mesotrione-achlorbenzene-triclopyr.
[0074] Example 2: A method for preparing a pesticide formulation containing mesotrione-ametryn-triclopyr, comprising the following steps:
[0075] S1. 2 g of wood powder, 14 mL of deionized water and 33 mL of acetone were added to an autoclave reactor, heated under reflux at 190 ° C for 120 min, extracted with dichloromethane at 35 ° C for 35 min, and then the obtained extract was collected by rotary evaporation and dried to obtain lignin powder;
[0076] S2. 1 mol of lignin powder and 2.5 mol of dimethyl sulfate were placed in a flask, heated under reflux at 75°C for 140 min, and then 10 mL of 2 mol / L hydrochloric acid solution was added, followed by washing twice with deionized water to obtain a mixture A;
[0077] S3. 1 mol of mixture A, 0.56 mol of diglycidyl ether and 0.04 mol of N,N-dimethylbenzylamine were heated to reflux at 95°C for 5.5 h, filtered, washed with a mixture of petroleum ether and deionized water in a volume ratio of 1:1.1, and dried at 55°C for 51 h to obtain modified lignin;
[0078] S4. 4.5 g of bark powder, 13 mL of deionized water and 34 mL of acetone were added to a three-necked flask, and heated under reflux at 48° C. for 100 min to obtain a tannin-rich liquid, and then the acetone was removed by evaporation, and deionized water was added to precipitate insoluble tannins, and then centrifuged and freeze-dried to obtain tannin powder;
[0079] S5. 1 g of modified lignin, 2.3 g of tannin powder, 16 mL of deionized water and 37 mL of acetone were placed in an ultrasonic bath and mixed evenly, and then 27 mL of deionized water was added using a constant flow pump, and the composite nanoparticles were collected by centrifugation and freeze drying;
[0080] S6. Add 5 g of the composite nanoparticles to 3.2 g of ethyl oleate additive and mix well to obtain additive A;
[0081] S7. After washing, crushing and drying the sugarcane straw, carbonizing it at 480°C, taking 5g of it and soaking it in 22g of 40% KOH solution by mass, stirring it for 12.5h, letting it stand for 22h, drying it at 115°C for 49h, cooling it, washing it twice with 1mol / L hydrochloric acid solution and deionized water, and then drying it at 65°C for 3.5h to obtain biochar;
[0082] S8. Inoculate the surface of TGY solid culture medium with Deinococcus by spreading method, and culture at 30°C for 56 hours, then inoculate in TGY liquid culture medium, culture at 30°C for 36 hours at a speed of 190 rpm, and finally centrifuge at 4500 rpm for 18 minutes, discard the supernatant, collect the bacteria, and prepare a bacterial suspension with sterile water to obtain Deinococcus agent;
[0083] S9. Add 10 g of biochar and 3.9 g of composite nanoparticles to 16.5 g of the Deinococcus agent, and place the conical flask in a constant temperature shaking incubator set at 30°C and 150 r / min for 22 h, take it out and let it stand for 2.5 h, filter it, rinse it with sterile water, and filter it to obtain additive B;
[0084] S10. 10.3 g of alkali lignin and 14 g of a 10% sodium hydroxide aqueous solution were stirred evenly, heated to 72 ° C, 1 g of formaldehyde was added dropwise, and the temperature was kept for 1.5 h. The temperature was again raised to 95 ° C and 5.7 g of anhydrous sodium sulfite was added. The reaction was kept for 2 h, washed twice with anhydrous ethanol, dialyzed, concentrated by rotary evaporation, and freeze-dried to obtain sulfomethylated lignin;
[0085] S11. After 11 g of sulfomethylated lignin was dissolved in water, sodium hydroxide was added to adjust the pH value to 11, the system temperature was raised to 80 ° C, 0.15 g of potassium iodide and 1.2 g of 1,6-dibromohexane were added, and after 5 h, it was washed twice with anhydrous ethanol, dialyzed, concentrated by rotary evaporation, and freeze-dried to obtain modified lignin sulfonate;
[0086] S12. 12 g of deionized water, 4 g of modified sodium lignin sulfonate, 4 g of sodium dodecyl sulfate, 0.2 g of silicone defoamer, and 0.5 g of urea were mixed and then 36 g of amethoxazole was added. The mixture was sheared for the first time at a speed of 5500 r / min for 13 min, and then poured into a sand mill containing zirconium beads and sanded for 1.5 h. After the particle size was sanded to less than 0.5 μm, the liquid was filtered out to obtain a mixture B;
[0087] S13. After evenly mixing 5g of mesotrione, 8g of butoxyethyl triclopyr and 37g of emulsifier 72-F, add mixture B, and perform a second shearing at a speed of 3000r / min for 15min. Then, add 0.5xanthan gum, 0.7g of kason and 4.5g of auxiliary agent, and perform a third shearing at a speed of 4500r / min for 10min. The mass ratio of auxiliary agent A to auxiliary agent B in the auxiliary agent is 30:10, so as to obtain a pesticide preparation containing mesotrione-achlorbenzene-triclopyr.
[0088] Example 3: A method for preparing a pesticide preparation containing mesotrione-ametryn-triclopyr, comprising the following steps:
[0089] S1. 3 g of wood powder, 15 mL of deionized water and 36 mL of acetone were added to an autoclave reactor, heated under reflux at 200 ° C for 130 min, extracted with dichloromethane at 40 ° C for 40 min, and then the obtained extract was collected by rotary evaporation and dried to obtain lignin powder;
[0090] S2. 1 mol of lignin powder and 2.7 mol of dimethyl sulfate were placed in a flask, heated under reflux at 78°C for 150 min, and then 13 mL of 2 mol / L hydrochloric acid solution was added, followed by washing twice with deionized water to obtain a mixture A;
[0091] S3. 1 mol of mixture A, 0.6 mol of diglycidyl ether and 0.05 mol of N,N-dimethylbenzylamine were heated to reflux at 100°C for 6 h, filtered, washed with a mixture of petroleum ether and deionized water in a volume ratio of 1:1.2, and dried at 60°C for 55 h to obtain modified lignin;
[0092] S4. 5 g of bark powder, 15 mL of deionized water and 38 mL of acetone were added to a three-necked flask, heated under reflux at 50° C. for 120 min to obtain a tannin-rich liquid, the acetone was removed by evaporation, deionized water was added to precipitate insoluble tannins, and then centrifuged and freeze-dried to obtain tannin powder;
[0093] S5. 1.3 g of modified lignin, 2.5 g of tannin powder, 18 mL of deionized water and 40 mL of acetone were placed in an ultrasonic bath and mixed evenly, and then 28 mL of deionized water was added using a constant flow pump, and the composite nanoparticles were collected by centrifugation and freeze drying;
[0094] S6. Add 7 g of the composite nanoparticles to 4.5 g of ethyl oleate additive and mix well to obtain additive A;
[0095] S7. After washing, crushing and drying the sugarcane straw, carbonizing it at 500°C, taking 5g of it and soaking it in 25g of a 40% KOH solution, stirring it for 13h, letting it stand for 20-24h, drying it at 120°C for 50h, cooling it, washing it twice with a 1mol / L hydrochloric acid solution and deionized water, and then drying it at 70°C for 4h to obtain biochar;
[0096] S8. Inoculate the surface of TGY solid culture medium with Deinococcus by coating method, and culture at 30°C for 72h, then inoculate in TGY liquid culture medium, culture at 30°C for 48h at a speed of 200rpm, and finally centrifuge at 5000rpm for 20min, discard the supernatant, collect the bacteria, and prepare a bacterial suspension with sterile water to obtain Deinococcus agent;
[0097] S9. Add 12 g of biochar and 4.5 g of composite nanoparticles to 18.7 g of the Deinococcus agent, and place the conical flask in a constant temperature shaking incubator set at 32° C. and 160 r / min for 24 h, take it out and let it stand for 3 h, filter it, rinse it with sterile water, and filter it to obtain additive B;
[0098] S10. 11 g of alkali lignin and 15 g of a 10% sodium hydroxide aqueous solution were stirred evenly, and 1 g of formaldehyde was added dropwise after the temperature was raised to 75 ° C. The temperature was kept for 2 h, and 6 g of anhydrous sodium sulfite was added after the temperature was raised to 97 ° C. The reaction was kept for 2.5 h, and the sulfomethylated lignin was obtained by washing twice with anhydrous ethanol, dialyzing, concentrating by rotary evaporation, and freeze-drying;
[0099] S11. After 12 g of sulfomethylated lignin was dissolved in water, sodium hydroxide was added to adjust the pH value to 11, the system temperature was raised to 83 ° C, 0.2 g of potassium iodide and 1.5 g of 1,6-dibromohexane were added, and after 5.5 h, it was washed twice with anhydrous ethanol, dialyzed, concentrated by rotary evaporation, and freeze-dried to obtain modified lignin sulfonate;
[0100] S12. 13 g of deionized water, 5 g of modified sodium lignin sulfonate, 5 g of sodium dodecyl sulfate, 0.3 g of silicone defoamer, and 0.7 g of urea were mixed and then 55 g of amethoxazole was added. The mixture was sheared for the first time at a speed of 6000 r / min for 15 min, and then poured into a sand mill containing zirconium beads and sanded for 2.0 h. After the particle size was sanded to less than 0.5 μm, the liquid was filtered out to obtain a mixture B;
[0101] S13. After uniformly mixing 6 g of mesotrione, 10 g of butoxyethyl triclopyr and 42 g of emulsifier 72-F, add mixture B, and perform a second shearing at a speed of 3500 r / min for 17 min. Then, add 0.8 xanthan gum, 1 g of kason and 5.2 g of auxiliary agent, and perform a third shearing at a speed of 5000 r / min for 13 min. The mass ratio of auxiliary agent A to auxiliary agent B in the auxiliary agent is 33:14, so as to obtain a pesticide preparation containing mesotrione-achlorbenzene-triclopyr.
[0102] Comparative Example 1:
[0103] Compared with Example 1, the composite nanoparticles were not added in the preparation process of the auxiliary agent A in this comparative example, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide preparation containing mesotrione-ametryn-triclopyr was obtained.
[0104] Comparative Example 2:
[0105] Compared with Example 1, this comparative example did not add methyl oleate adjuvant during the preparation of adjuvant A, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide preparation containing mesotrione-ametryn-triclopyr was obtained.
[0106] Comparative Example 3:
[0107] Compared with Example 1, in this comparative example, the auxiliary agent A was not added during the preparation process of the pesticide preparation containing mesotrione-ametryn-triclopyr, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide preparation containing mesotrione-ametryn-triclopyr was obtained.
[0108] Comparative Example 4:
[0109] Compared with Example 1, in this comparative example, the auxiliary agent B was not added during the preparation process of the pesticide preparation containing mesotrione-ametryn-triclopyr, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide preparation containing mesotrione-ametryn-triclopyr was obtained.
[0110] Comparative Example 5:
[0111] Compared with Example 1, biochar was not added during the preparation of the adjuvant B in this comparative example, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide preparation containing mesotrione-ametryn-triclopyr was obtained.
[0112] Comparative Example 6:
[0113] Compared with Example 1, this comparative example only replaces "modified lignin" with "lignin", and the remaining steps and parameters are the same, which will not be repeated in this comparative example. Finally, a pesticide preparation containing mesotrione-ametryn-triclopyr is obtained.
[0114] Comparative Example 7:
[0115] Compared with Example 1, this comparative example only replaces "modified lignin sulfonate" with "lignin sulfonate", and the remaining steps and parameters are the same, which will not be repeated in this comparative example. Finally, a pesticide preparation containing mesotrione-ametryn-triclopyr is obtained.
[0116] Comparative Example 8:
[0117] Compared with Example 1, no adjuvant was added in the preparation process of the pesticide preparation containing mesotrione-ametryn-triclopyr in this comparative example, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide preparation containing mesotrione-ametryn-triclopyr was obtained.
[0118] Comparative Example 9:
[0119] Compared with Example 1, in this comparative example, no Deinococcus aureus agent was added during the preparation process of the pesticide preparation containing mesotrione-ametryn-triclopyr, and the remaining steps and parameters were the same, which will not be repeated in this comparative example. Finally, a pesticide preparation containing mesotrione-ametryn-triclopyr was obtained.
[0120] Performance Test:
[0121] Thermal storage stability:
[0122] According to the determination method of GB / T19136-2003, the pesticide preparation containing mesotrione-ametryn-triclopyr prepared in Example 1 to Example 3 and Comparative Example 1 to Comparative Example 9 was sealed and placed in a thermostatic box at (54±2)°C for 14 days, then taken out and cooled to room temperature. The technical indicators such as appearance, fluidity, dispersibility, active ingredient content, suspension rate and pourability were analyzed and tested and recorded. If the indicators did not change significantly before and after hot storage, the hot storage stability was considered to be qualified; if the appearance and suspension rate did not change significantly before and after storage, the cold storage stability was considered to be qualified;
[0123] Cold storage stability:
[0124] According to the determination method of GB / T19137-2003, the pesticide formulation containing mesotrione-ametryn-triclopyr prepared in Examples 1 to 3 and Comparative Examples 1 to 9 was placed in a (0±2)°C refrigerator for 1 hour, and the appearance was observed for changes. Then, the formulation was further stored in a (0±2)°C refrigerator for 7 days. If the appearance and suspension rate did not change significantly before and after storage, the cold storage stability was considered to be qualified.
[0125] Suspension rate performance test:
[0126] According to the GB / T14825-2006 test standard, 5 g of the pesticide preparation containing mesotrione-ametryn-triclopyr prepared in Examples 1 to 3 and Comparative Examples 1 to 9 were weighed into a 200 mL clean measuring cylinder, standard hard water was added to the scale line, the ground stopper was covered, and after sufficient shaking for 3 minutes, the stopper was opened and placed in a water bath for heating for 30 minutes, and the heating temperature was controlled at (30±2)°C. 9 / 10 of the liquid was precipitated with a pipette. During this process, the pipette should not be inserted into the bottom of the measuring cylinder, and the measuring cylinder should not be shaken during the whole process. All the remaining contents in the measuring cylinder were transferred to a clean beaker for drying and weighing;
[0127] Suspension rate calculation formula:
[0128]
[0129] Wherein, m is the weighed mass of the sample, g; w is the percentage of the active ingredient of the pesticide, %; m1 is the mass of the beaker, g; m2 is the total mass after drying, g.
[0130] Weed control effect:
[0131] A sugarcane field with normal fertility, weeds at the 3-5 leaf stage when applying the pesticide, and no other herbicides were used before applying the pesticide, was divided into 11 groups to treat the sugarcane field with the pesticide preparations containing mesotrione-ametryn-triclopyr prepared in Examples 1 to 3 and Comparative Examples 1 to 9, each treatment was repeated 4 times, and the area of each plot was 20 m2 , randomized block arrangement, on a sunny day, directional spraying was used to spray the weeds on the stems and leaves once, avoiding contact of the liquid with the sugarcane leaves, and the water was diluted to 895.52 L·hm according to the experimental measurement. -2 , and a blank control group was set up to spray the same amount of water. Five points were randomly selected from each plot, with a 0.2 m 2 , investigate the plant control effect once at 15d and 30d after application;
[0132] Calculation method of drug efficacy:
[0133]
[0134] Table 1
[0135] project Thermal storage stability Cold storage stability Suspension rate / % Example 1 qualified qualified 98.5 Example 2 qualified qualified 99.2 Example 3 qualified qualified 96.3 Comparative Example 1 Failure Failure 73.9 Comparative Example 2 Failure Failure 75.1 Comparative Example 3 Failure Failure 68.9 Comparative Example 4 Failure Failure 72.5 Comparative Example 5 qualified qualified 79.2 Comparative Example 6 qualified qualified 78.6 Comparative Example 7 qualified qualified 82.9 Comparative Example 8 Failure Failure 63.5 Comparative Example 9 qualified qualified 83.5
[0136] Table 2
[0137]
[0138]
[0139] Data Analysis:
[0140] As can be seen from Table 1, the pesticide preparation containing mesotrione-ametryn-triclopyr prepared by the present invention has better herbicidal performance. This may be because the additive A added in the present invention is obtained by mixing composite nanoparticles with methyl oleate additives. The modified lignin and tannin powder contained therein have good ultraviolet shielding performance. By preparing them in nano form, their biocompatibility and dispersibility in the pesticide preparation can be enhanced. The methyl oleate additive dissolves the wax on the surface of the weeds, so that the herbicide can better wet the leaf surface and then penetrate into the inside of the leaf to exert the weeding effect. The molecules of the composite nanoparticles contain abundant oxygen-containing groups. On the one hand, under the action of the modified lignin sulfonate dispersant, they may cross-link with the methyl oleate additive, thereby enhancing the adhesion of the composite nanoparticles on the leaf surface, and the formed ultraviolet shielding layer can fit closely with the leaf surface. On the other hand, the oxygen-containing groups in the composite nanoparticles will form molecular bonds with the modified lignin sulfonate dispersant. The adjuvant B is prepared from biochar, composite nanoparticles and azotobacter, wherein the azotobacter absorbs ultraviolet rays and converts them into heat, thereby increasing the temperature of the weed leaf surface, which is not conducive to the growth of weeds in a high temperature environment; and the biochar can further improve the stability and dispersibility of the adjuvant, and can also adsorb the herbicide, reduce the leaching and migration of the herbicide, and maximize the utilization of the herbicide; through the compound use of adjuvant A and adjuvant B, the pesticide preparation prepared by the present invention has good wettability, so that the three herbicides of mesotrione, triclopyr butoxyethyl and amethoxazole can be better attached to the leaf surface and absorbed by the weeds, thereby exerting a chemical weed control effect; the ultraviolet shielding layer on the leaf surface can not only prevent the herbicide from photodegradation and then becoming ineffective, but also directly hinder the photosynthesis of the weeds through the physical barrier effect, thereby realizing the efficient utilization of the herbicide and having a good control effect on the annual weeds in the sugarcane field;
[0141] As for Comparative Example 1, since the composite nanoparticles were not added in the preparation process of the auxiliary agent A, it can be seen from Table 1 that its utilization rate is worse than that of Example 1. This may be because the composite nanoparticles themselves have good ultraviolet shielding properties, and can form a layer of ultraviolet shielding layer on the weed leaf surface with the methyl oleate auxiliary agent, which can not only protect the activity of the original drug, but also directly hinder the photosynthesis of the weeds, play a dual weeding effect, and improve the utilization rate of the herbicide; as for Comparative Example 2, since the methyl oleate auxiliary agent was not added in the preparation process of the auxiliary agent A, it can be seen from Table 1 that its utilization rate is worse than that of Example 1. This may be because the methyl oleate auxiliary agent can reduce the surface tension, reduce the contact angle, and enhance the wettability of the pesticide. At the same time, it may also react with the composite nanoparticles, further Improve the utilization rate of pesticides; Comparative Example 3 does not add auxiliary agent A during the preparation of the pesticide formulation containing mesotrione-ametryn-triclopyr. As can be seen from Table 1, its utilization rate is worse than that of Example 1. This may be due to the fact that auxiliary agent A improves the wettability and dispersibility of the original drug, prevents the photodegradation of the original drug, and directly hinders the photosynthesis of plants. Effectively improve the utilization rate of the herbicide; Comparative Example 4 does not add auxiliary agent B during the preparation of the pesticide formulation containing mesotrione-ametryn-triclopyr. As can be seen from Table 1, its utilization rate is worse than that of Example 1. This may be due to the fact that auxiliary agent B effectively improves the herbicide from three aspects: reducing the leaching and migration of the herbicide, preventing the photodegradation of the original drug, and directly hindering the photosynthesis of plants. The utilization rate of the agent; Comparative Example 5 does not add biochar during the preparation of the auxiliary agent B. As can be seen from Table 1, its utilization rate is worse than that of Example 1. This may be because biochar can not only provide good adsorption sites for the Deinococcus agent, but also adsorb the herbicide to reduce its loss rate due to rainwater erosion; Comparative Example 6 replaces "modified lignin" with "lignin". As can be seen from Table 1, its utilization rate is worse than that of Example 1. This may be because the phenolic active sites of lignin in the modified lignin are reduced, which increases its hydrophobicity, thereby increasing the surface tension and contact angle, enhancing the wettability of the original drug on the leaf surface, and facilitating the uniform spreading of the herbicide on the weeds, thereby improving the utilization rate; Comparative Example 7 replaces "modified lignin sulfonate" with "lignin sulfonate" "Acid salt", as can be seen from Table 1, its utilization rate is worse than that of Example 1. This may be because after the sulfomethylated lignin is grafted with an alkyl bridge, the interaction force between lignin molecules is enhanced, which increases the distance between molecules, thereby reducing the aggregation between molecules, and the molecules have a certain hydrophobicity, which can interact with the wax layer on the leaf surface, reduce the surface tension, and improve the dispersibility, which is helpful to improve the utilization rate of the herbicide; Comparative Example 8 does not add auxiliary agents during the preparation process of the pesticide preparation containing mesotrione-ametryn-triclopyr. As can be seen from Table 1, its utilization rate is worse than that of Example 1. This may be due to the anti-degradation and anti-leaching effects of auxiliary agents A and auxiliary agent B on the original drug and the direct obstruction of leaf photosynthesis, thereby improving the overall utilization rate of the herbicide;Comparative Example 9 did not add the Deinococcus aureus agent during the preparation of the pesticide formulation containing mesotrione-ametryn-triclopyr. As can be seen from Table 1, its utilization rate is worse than that of Example 1. This may be because the Deinococcus aureus agent absorbs ultraviolet rays and converts them into heat, thereby increasing the temperature of the weed leaf surface, which is not conducive to the growth of weeds in a high temperature environment. At the same time, it directly hinders the photosynthesis of plants, thereby increasing the overall utilization rate of the herbicide. ;
[0142] Those skilled in the art should understand that the discussion of any of the above embodiments is merely illustrative and is not intended to imply that the scope of the present invention is limited to these examples. Under the concept of the present invention, the technical features in the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity.
[0143] The present invention is intended to cover all such substitutions, modifications and variations that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. A pesticide preparation containing mesotrione-ametryn-triclopyr, characterized in that: Prepared from the following raw materials by weight: 3-6 parts of mesotrione, 27.5-55 parts of ametryn, 5-10 parts of butoxyethyl triclopyr, 32-42 parts of emulsifier, 3-5 parts of wetting agent, 3-5 parts of dispersant, 0.3-0.8 parts of thickener, 0.4-0.7 parts of antifreeze agent, 0.1-0.3 parts of organosilicon defoamer, 0.5-1 parts of preservative, 3.4-5.2 parts of auxiliary agent, 10-13 parts of deionized water; The auxiliary agent is obtained by mixing auxiliary agent A and auxiliary agent B in a mass ratio of 27-33:8-14; The auxiliary agent A is obtained by mixing composite nanoparticles and methyl oleate auxiliary agent in a mass ratio of 3-7:1.8-4.5; The auxiliary agent B is prepared from biochar, composite nanoparticles and Deinococcus agent; The mass ratio of the biochar, the composite nanoparticles and the Deinococcus agent is 8-12:3.3-4.5:15.5-18.7; The composite nanoparticles are obtained by mixing tannin powder and modified lignin in a mass ratio of 0.8-1.3:2-2.
5.
2. The pesticide preparation containing mesotrione-ametryn-triclopyr according to claim 1, characterized in that: The preparation method of the modified lignin is as follows: Step A1. Add wood powder, deionized water and acetone into an autoclave reactor, heat and reflux at 185-200°C for 110-130 min, extract with dichloromethane at 30-40°C for 30-40 min, and then collect the obtained extract by rotary evaporation and dry to obtain lignin powder; Step A2. Place lignin powder and dimethyl sulfate in a flask, heat and reflux at 72-78° C. for 130-150 min, add a 2 mol / L hydrochloric acid solution, and then wash twice with deionized water to obtain a mixture A; Step A3. The mixture A, diglycidyl ether and N,N-dimethylbenzylamine are heated to reflux, filtered, washed with a mixture of petroleum ether and deionized water, and dried at 50-60° C. for 48-55 hours to obtain modified lignin.
3. The pesticide preparation containing mesotrione-ametryn-triclopyr according to claim 2, characterized in that: The ratio of wood powder, deionized water and acetone in step A1 is 2-3 g: 12-15 mL: 30-36 mL; The ratio of lignin to dimethyl sulfate and hydrochloric acid solution in step A2 is 1 mol: 2.4-2.7 mol: 8-13 mL; In step A3, the molar ratio of the mixture A to diglycidyl ether and N,N-dimethylbenzylamine is 1:0.4-0.6:0.02-0.05; The volume ratio of petroleum ether to deionized water in the petroleum ether-deionized water mixture is 1:1-1.2; The temperature during the heating reflux is 90-100° C. and the time is 5-6 hours.
4. The pesticide preparation containing mesotrione-ametryn-triclopyr according to claim 1, characterized in that: The preparation method of the auxiliary agent A is as follows: Step B1. Add bark powder, deionized water and acetone into a three-necked flask, heat and reflux at 45-50° C. for 90-120 min to obtain a tannin-rich liquid, remove the acetone by evaporation, add deionized water to precipitate insoluble tannin, and then centrifuge and freeze-dry to obtain tannin powder; Step B2. The modified lignin, tannin powder, deionized water and acetone were placed in an ultrasonic bath and mixed evenly, and then 25-28 mL of deionized water was added using a constant flow pump, and the composite nanoparticles were collected by centrifugation and freeze drying; Step B3. adding the composite nanoparticles to the ethyl oleate additive and mixing them evenly to obtain additive A; The ratio of the bark powder, deionized water and acetone in step B1 is 4-5 g: 12-15 mL: 30-38 mL; The usage ratio of the modified lignin, tannin powder, deionized water and acetone in step B2 is 0.8-1.3 g: 2-2.5 g: 15-18 mL: 35-40 mL.
5. The pesticide preparation containing mesotrione-ametryn-triclopyr according to claim 1, characterized in that: The preparation method of the auxiliary agent B is as follows: Step C1. After washing, crushing and drying the sugarcane straw, carbonizing it at 450-500°C, taking 5g of it and soaking it in 20-25g of a 40% KOH solution by mass, stirring it for 12-13h, letting it stand for 20-24h, drying it at 110-120°C for 48-50h, cooling it, washing it twice with a 1mol / L hydrochloric acid solution and deionized water, and then drying it at 60-70°C for 3-4h to obtain biochar; Step C2. Inoculate the surface of TGY solid culture medium with Deinococcus by coating method, and culture at 30°C for 48-72h, then inoculate in TGY liquid culture medium, culture at 30°C for 24-48h at a speed of 180-200rpm, and finally centrifuge at 4000-5000rpm for 15-20min, discard the supernatant, collect the bacteria, and prepare a bacterial suspension with sterile water to obtain Deinococcus agent; Step C3. Add biochar and composite nanoparticles to the Deinococcus agent, and place the conical flask in a constant temperature shaking incubator set at a temperature of 28-32°C and a rotation speed of 130-160 r / min for 20-24 hours, take it out and let it stand for 2-3 hours, filter it, rinse it with sterile water, and filter it to obtain additive B; The TGY solid culture medium in step C2 is formulated as follows: 0.5% tryptone, 0.3% yeast extract, 0.1% glucose, 1.5% agar, and a pH of 7.0-7.2; The formula of the TGY liquid culture medium is: 0.5% tryptone, 0.3% yeast extract, 0.1% glucose, and pH is 7.0-7.
2.
6. The pesticide preparation containing mesotrione-ametryn-triclopyr according to claim 1, characterized in that: The emulsifier is emulsifier 72-F; The wetting agent is any one of sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, and sodium lauryl sulfate; The dispersant is a modified lignin sulfonate; The thickener is any one of xanthan gum, magnesium aluminum silicate, polyvinyl alcohol and organic bentonite; The antifreeze agent is any one of ethylene glycol, glycerol, polyethylene glycol and urea; The preservative is Kathon.
7. The pesticide preparation containing mesotrione-ametryn-triclopyr according to claim 6, characterized in that: The preparation method of the modified lignin sulfonate is as follows: Step D1. The alkali lignin and a 10% sodium hydroxide aqueous solution are uniformly stirred, the temperature is raised to 70-75°C, formaldehyde is added dropwise, and the temperature is kept for 1.5-2 hours. The temperature is raised to 92-97°C again, anhydrous sodium sulfite is added, and the temperature is kept for 2-2.5 hours. The mixture is washed twice with anhydrous ethanol, dialyzed, concentrated by rotary evaporation, and freeze-dried to obtain sulfomethylated lignin; Step D2. After dissolving the sulfomethylated lignin in water, add sodium hydroxide to adjust the pH value to 11, increase the system temperature to 78-83°C, add potassium iodide and 1,6-dibromohexane, wash twice with anhydrous ethanol after 4.5-5.5 hours, dialyze, concentrate by rotary evaporation, and freeze-dry to obtain modified lignin sulfonate.
8. The pesticide preparation containing mesotrione-ametryn-triclopyr according to claim 7, characterized in that: The mass ratio of alkali lignin, sodium hydroxide aqueous solution, formaldehyde and anhydrous sodium sulfite in step D1 is 9.5-11:13-15:1:5.3-6; The mass ratio of the sulfomethylated lignin, potassium iodide and 1,6-dibromohexane in step D2 is 10-12: 0.1-0.2:0.8-1.5。 9. A method for preparing a pesticide preparation containing mesotrione-ametryn-triclopyr according to any one of claims 1 to 8, characterized in that: The following steps are involved: Step S1. After deionized water, dispersant, wetting agent, silicone defoamer and antifreeze are mixed evenly, ametryn is added, and the mixture is sheared for the first time. The mixture is then poured into a sand mill containing zirconium beads and sand milled for 1.5-2.0 hours. After the particle size is sand milled to less than 0.5 μm, the liquid medicine is filtered out to obtain a mixture B. Step S2. After mesotrione, butoxyethyl triclopyr and an emulsifier are uniformly mixed, mixture B is added, and a second shearing is performed. After a thickener, a preservative and an adjuvant are added, a third shearing is performed to obtain a pesticide preparation containing mesotrione-ametryn-triclopyr.
10. The method for preparing the pesticide preparation containing mesotrione-ametryn-triclopyr according to claim 9, characterized in that: The speed of the first shearing in step S1 is 5000-6000 r / min, and the time is 10-15 min; The speed of the second shearing in step S2 is 3000-3500 r / min, and the time is 12-17 min; The speed of the third shearing in step S2 is 4500-5000 r / min, and the time is 8-13 min.
Citation Information
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