CN113016809A - Compound herbicide for sugarcane based on triclopyr and diuron - Google Patents
Compound herbicide for sugarcane based on triclopyr and diuron Download PDFInfo
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- CN113016809A CN113016809A CN202110267033.2A CN202110267033A CN113016809A CN 113016809 A CN113016809 A CN 113016809A CN 202110267033 A CN202110267033 A CN 202110267033A CN 113016809 A CN113016809 A CN 113016809A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/30—Derivatives containing the group >N—CO—N aryl or >N—CS—N—aryl
Abstract
The invention discloses a triclopyr and diuron-based compound herbicide for sugarcane, which comprises the following raw materials of, by weight, 1-60% of triclopyr, 1-30% of diuron, 3-8% of an auxiliary agent and the balance of a carrier, wherein the dosage form of the triclopyr and diuron-based compound herbicide for sugarcane is one of a dispersible suspending agent, a wettable powder and a water dispersible granule. The amphiphilic chitosan surfactant is obtained by performing carboxylation modification and alkylation modification on chitosan, can be effectively adsorbed on the surfaces of pesticide particles, and can be well dispersed in water, so that the dispersibility of the pesticide is improved, and the effect of the pesticide is improved; the chitosan has wide source, is biodegradable and has good environmental protection performance; meanwhile, the invention utilizes a compounding technology, slows down the generation of drug resistance and widens the weeding spectrum of the herbicide.
Description
Technical Field
The invention belongs to the technical field of pesticide processing, and particularly relates to a triclopyr and diuron-based compound herbicide for sugarcane.
Background
Sugarcane is the economic crop with the largest planting area in Guangxi regions, the annual planting area is about 18000 mu of a thousand, the sugarcane is mainly distributed in the middle, south and southwest of Guangxi, and the planting time is generally concentrated in winter and spring. At the moment, the temperature is low, drought and rain are low, the mulching film can play a good role in warming and preserving soil moisture, the emergence rate of the sugarcane is effectively improved, but the high-temperature and high-humidity environment under the film is also beneficial to the growth of weeds, and the growth of the sugarcane is seriously influenced if the film is not controlled in time, so that the yield of the sugarcane is reduced. Therefore, before mulching the mulching film, the herbicide is generally sprayed to achieve the purpose of preventing and killing weeds under the mulching film, but the method not only easily destroys the sealing layer to influence the weeding effect, but also causes the pesticide to be drifted into the surrounding environment in the spraying process of the herbicide to cause adverse effects on the environment. In addition, the tillering stage of the sugarcane is also affected by weeds, so that the yield of the sugarcane is reduced. If the effective control is not carried out, the yield of the sugarcane is reduced by 20-30 percent generally, and the yield is reduced by more than 50 percent in serious cases until the sugarcane is completely dead. Therefore, the prevention and control of weeds in the sugarcane field have important effects on guaranteeing the production of the sugarcane and increasing the income of sugarcane farmers. However, the existing herbicide for sugarcane has the following problems that the varieties and dosage forms of the chemical herbicide adopted at present in China are seriously aged, the weed resistance is increased year by year, so that the dosage of the traditional herbicide is increased extremely quickly, the dosage per mu is increased by more than 50 percent compared with that of about 2000 years, and the cost is greatly increased; the common herbicide for sugarcane at present is wettable powder, generates a large amount of dust in the production and use processes, and is not beneficial to body health and environmental protection; the dilution ratio of the common sugarcane field herbicide is 300-500, the common sugarcane field herbicide is easy to stratify when mixed with water for spraying, and some solid fillers are deposited to easily block spraying equipment; when low-capacity equipment is used for spraying, the diluted liquid medicine is diluted by 10-30 times, the liquid medicine cannot be uniformly dispersed, and the spraying equipment is seriously blocked.
Triclopyr is a class of systemic, conductive, low toxicity herbicide in picoxycarboxylic acids, also known as Geranium, triclopyr. Absorbed by leaf surface and root system of plant, and conducted to whole plant in plant body, resulting in malformation of root, stem and leaf, depletion of stored substance, embolism or rupture of vascular bundle, and gradual death of plant. The weeding composition is suitable for weeding, killing irrigation, maintaining fire lines, supporting and cultivating pine trees and forest stand transformation before forest forestation, and is used for preventing and killing broad leaf weeds and woody plants in non-cultivated land. Triclopyr can be decomposed by soil microorganisms in soil with a half-life of 30-46 days.
Diuron is a systemic herbicide and has certain contact killing performance. After being absorbed into human plants by roots and leaves of the plants, the plants inhibit photosynthesis of the plants, so that the leaves turn yellow and die finally. Can be used for dry land plants such as cotton, corn, peanut, sugarcane, fruit tree, tea tree, rubber tree, etc., and can prevent and kill annual weeds such as crabgrass, Echinochloa crusgalli, green bristlegrass, polygonum, chenopodium album, Cyperus rotundus, etc. It also has good control effect on perennial weeds such as bermuda grass, cyperus rotundus and the like.
Accordingly, the present invention provides a compound herbicide for sugarcane based on triclopyr and diuron to solve the above-mentioned problems.
Disclosure of Invention
The invention aims to provide a compound herbicide for sugarcane based on triclopyr and diuron, which is used for solving the problems of aging, high drug resistance and high weeding cost of the herbicide for sugarcane.
The purpose of the invention can be solved by the following technical scheme:
a composite herbicide based on triclopyr and diuron for sugarcane comprises the following raw materials, by weight, 1-60% of triclopyr, 1-30% of diuron, 3-8% of an auxiliary agent, and the balance of a carrier.
Furthermore, the dosage form of the compound herbicide for sugarcane based on triclopyr and diuron is one of dispersible suspending agent, wettable powder and water dispersible granule.
The carrier can be one or a mixture of more of deionized water, an organic solvent or a filler in any ratio according to the dosage form, the organic solvent is one or a mixture of more of toluene, ethanol, ethanolamine, propanol, butanol and ethylene glycol in any ratio, and the filler is one or a mixture of more of diatomite, white carbon black, starch and light calcium carbonate in any ratio.
Further, the auxiliary agent is a mixture of amphiphilic chitosan, sodium carboxymethyl cellulose, epoxidized soybean oil and propanol in any ratio.
Further, the preparation method of the amphiphilic chitosan comprises the following steps:
step A, dissolving chitosan in 1% acetic acid water solution, filtering insoluble substances, adding sodium hydroxide into the dissolved filtrate under stirring to obtain white precipitate, and filtering; soaking the filter cake in distilled water, adjusting the pH of the solution to 6-7 with hydrochloric acid, and filtering; washing with distilled water for multiple times, precipitating with acetone, filtering, and drying the filter cake in a vacuum drying oven at 50-60 deg.C for 1h to obtain treated chitosan; filling the treated chitosan into a reaction bottle with a stirrer, adding sodium hydroxide solution with the mass concentration of 35% and isopropanol, stirring to react for 50min, slowly dropwise adding monochloroacetic acid, completing the dropwise adding within 30min, heating to 60-65 ℃, continuing to stir to react for 3h, neutralizing to be neutral by using dilute hydrochloric acid after the reaction is stopped, precipitating and filtering a product by using acetone, washing for 2-3 times by using 85% methanol solution, washing for 1 time by using anhydrous methanol, precipitating and filtering by using acetone, and placing a filter cake at 30-35 ℃ for vacuum drying to obtain carboxymethyl chitosan;
b, dissolving the carboxymethyl chitosan obtained in the step A in a water-alcohol solution, stirring and swelling for 2-3h at 30-35 ℃, adding phosphotungstic acid and hydrogen peroxide with the mass concentration of 30%, performing reflux reaction for 1-3h at 60-70 ℃, performing ultrasonic treatment for 30min, precipitating the product with propanol, filtering, washing for 2-3 times with 85% methanol solution, washing for 1 time with anhydrous methanol, precipitating with acetone, filtering, and performing vacuum drying on the filter cake at 30-35 ℃ to obtain the treated carboxymethyl chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4: 1;
and step C, putting the carboxymethyl chitosan treated in the step B into a water-alcohol solution, adding allyl glycidyl ether, uniformly stirring, reacting for 2 hours at the temperature of 80-95 ℃, adding dodecyl trimethoxy silane, reacting for 3-5 hours at the temperature of 70-80 ℃, precipitating the product with propanol, filtering, washing the product with 85% methanol solution for 2-3 times, washing with anhydrous methanol for 1 time, precipitating with acetone, filtering, and drying the filter cake in vacuum at the temperature of 30-35 ℃ to obtain the amphiphilic chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4: 1.
Further, in the step A, the dosage ratio of the chitosan, the acetic acid aqueous solution, the sodium hydroxide and the hydrochloric acid is 10-15g: 500-; the usage ratio of the treated chitosan, the sodium hydroxide solution, the isopropanol and the monochloroacetic acid is 5-12g, 30-60ml, 20-30ml and 3-6 g.
Further, the dosage ratio of the carboxymethyl chitosan, the hydroalcoholic solution, the phosphotungstic acid and the hydrogen peroxide in the step B is 5-9g: 100-.
Furthermore, the dosage ratio of the carboxymethyl chitosan, the hydroalcoholic solution, the allyl glycidyl ether and the dodecyl trimethoxy silane after being treated in the step C is 6-13g, 80-120ml, 3-6g and 3-6 g.
The invention has the beneficial effects that:
1. according to the invention, the amphiphilic chitosan surfactant is obtained by performing carboxylation modification and alkylation modification on chitosan, can be effectively adsorbed on the surface of pesticide particles, and can form a good adsorption effect with the filler, and the amphiphilic chitosan can be well dispersed in water, so that the dispersibility of the pesticide or the filler is improved, and the effect of the pesticide is improved; the chitosan has wide source, is biodegradable and has good environmental protection performance;
2. the herbicide for the sugarcane is compounded by utilizing the triclopyr and the diuron, so that the dosage form of the herbicide for the sugarcane is increased, the generation of drug resistance is slowed down by utilizing a compounding technology, the effective dose of a pesticide is reduced, and the weeding spectrum of the herbicide is widened.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
a composite herbicide based on triclopyr and diuron for sugarcane is a dispersible suspending agent and comprises the following raw materials, by weight, 20% of triclopyr, 15% of diuron, 3% of an auxiliary agent and the balance of propanol.
Wherein the auxiliary agent is a mixture of amphiphilic chitosan, sodium carboxymethylcellulose, epoxidized soybean oil and propanol in a mounting mass ratio of 1.5:15:0.5: 0.5.
The preparation method of the amphiphilic chitosan comprises the following steps:
step A, dissolving chitosan in 1% acetic acid water solution, filtering insoluble substances, adding sodium hydroxide into the dissolved filtrate under stirring to obtain white precipitate, and filtering; soaking the filter cake in distilled water, adjusting the pH of the solution to 7 with hydrochloric acid, and filtering; washing with distilled water for multiple times, precipitating with acetone, filtering, and drying the filter cake in a vacuum drying oven at 50 deg.C for 1h to obtain treated chitosan; filling the treated chitosan into a reaction bottle with a stirrer, adding a sodium hydroxide solution with the mass concentration of 35% and isopropanol, stirring to react for 50min, slowly dropwise adding monochloroacetic acid, completing the dropwise adding within 30min, heating to 60 ℃, continuing to stir to react for 3h, neutralizing to be neutral by using dilute hydrochloric acid after the reaction is stopped, precipitating the product by using acetone, filtering, washing for 2 times by using an 85% methanol solution, washing for 1 time by using anhydrous methanol, precipitating by using acetone, filtering, and placing a filter cake at 30 ℃ for vacuum drying to obtain carboxymethyl chitosan, wherein the dosage ratio of the chitosan, an acetic acid aqueous solution, the sodium hydroxide and the hydrochloric acid in the step A is 10g:500ml:1 mol; the using ratio of the treated chitosan to the sodium hydroxide solution to the treated isopropanol to the treated monochloroacetic acid is 5g to 30ml to 20ml to 3 g;
b, dissolving the carboxymethyl chitosan obtained in the step A in a water-alcohol solution, stirring and swelling for 2 hours at 30 ℃, then adding phosphotungstic acid and hydrogen peroxide with the mass concentration of 30%, carrying out reflux reaction for 1 hour at 70 ℃, carrying out ultrasonic treatment for 30min, then precipitating the product by using propanol, filtering, washing for 2 times by using a methanol solution with the concentration of 85%, washing for 1 time by using anhydrous methanol, precipitating by using acetone, filtering, and carrying out vacuum drying on a filter cake at 30 ℃ to obtain the treated carboxymethyl chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4:1, and the dosage ratio of the carboxymethyl chitosan, the water-alcohol solution, the phosphotungstic acid and the hydrogen peroxide is 5g:100mL:3mg:3 mL;
and step C, putting the carboxymethyl chitosan treated in the step B into a water-alcohol solution, adding allyl glycidyl ether, uniformly stirring, reacting for 2 hours at 95 ℃, adding dodecyl trimethoxy silane, reacting for 3 hours at 70 ℃, precipitating the product with propanol, filtering, washing with 85% methanol solution for 2 times, washing with anhydrous methanol for 1 time, precipitating with acetone, filtering, and drying the filter cake in vacuum at 30 ℃ to obtain the amphiphilic chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4:1, and the dosage ratio of the carboxymethyl chitosan, the water-alcohol solution, the allyl glycidyl ether and the dodecyl trimethoxy silane after being treated in the step C is 6g:80ml:3g:3 g.
Dissolving triclopyr, diuron, propanol and an auxiliary agent in the formula into a uniform oil phase; under high-speed stirring, the triclopyr and diuron are mixed to prepare the sugarcane composite dispersible suspending agent.
Example 2:
a compound herbicide based on triclopyr and diuron for sugarcane is a suspending agent and comprises the following raw materials, by weight, 30% of triclopyr, 10% of diuron, 6% of an auxiliary agent and the balance of deionized water.
Wherein the auxiliary agent is amphiphilic chitosan, sodium carboxymethylcellulose, epoxidized soybean oil and propanol according to the mass ratio of 1:1:1: 1.
The preparation method of the amphiphilic chitosan comprises the following steps:
step A, dissolving chitosan in 1% acetic acid water solution, filtering insoluble substances, adding sodium hydroxide into the dissolved filtrate under stirring to obtain white precipitate, and filtering; soaking the filter cake in distilled water, adjusting the pH of the solution to 7 with hydrochloric acid, and filtering; washing with distilled water for multiple times, precipitating with acetone, filtering, and drying the filter cake in a vacuum drying oven at 50 deg.C for 1h to obtain treated chitosan; filling the treated chitosan into a reaction bottle with a stirrer, adding a sodium hydroxide solution with the mass concentration of 35% and isopropanol, stirring to react for 50min, slowly dropwise adding monochloroacetic acid, completing the dropwise adding within 30min, heating to 60 ℃, continuing to stir to react for 3h, neutralizing to be neutral by using dilute hydrochloric acid after the reaction is stopped, precipitating the product by using acetone, filtering, washing for 2 times by using an 85% methanol solution, washing for 1 time by using anhydrous methanol, precipitating by using acetone, filtering, and placing a filter cake at 30 ℃ for vacuum drying to obtain carboxymethyl chitosan, wherein the dosage ratio of the chitosan, an acetic acid aqueous solution, the sodium hydroxide and the hydrochloric acid in the step A is 12g:650ml:1 mol; the using ratio of the treated chitosan to the sodium hydroxide solution to the treated isopropanol to the treated monochloroacetic acid is 6g to 40ml to 25ml to 4 g;
b, dissolving the carboxymethyl chitosan obtained in the step A in a water-alcohol solution, stirring and swelling for 2 hours at 30 ℃, then adding phosphotungstic acid and hydrogen peroxide with the mass concentration of 30%, carrying out reflux reaction for 1 hour at 70 ℃, carrying out ultrasonic treatment for 30min, then precipitating the product by using propanol, filtering, washing for 2 times by using a methanol solution with the concentration of 85%, washing for 1 time by using anhydrous methanol, precipitating by using acetone, filtering, and carrying out vacuum drying on a filter cake at 30 ℃ to obtain the treated carboxymethyl chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4:1, and the dosage ratio of the carboxymethyl chitosan, the water-alcohol solution, the phosphotungstic acid and the hydrogen peroxide is 7g:130mL:4mg:4 mL;
and step C, putting the carboxymethyl chitosan treated in the step B into a water-alcohol solution, adding allyl glycidyl ether, uniformly stirring, reacting for 2 hours at 95 ℃, adding dodecyl trimethoxy silane, reacting for 3 hours at 70 ℃, precipitating the product with propanol, filtering, washing with 85% methanol solution for 2 times, washing with anhydrous methanol for 1 time, precipitating with acetone, filtering, and drying the filter cake in vacuum at 30 ℃ to obtain the amphiphilic chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4:1, and the dosage ratio of the carboxymethyl chitosan, the water-alcohol solution, the allyl glycidyl ether and the dodecyl trimethoxy silane after being treated in the step C is 10g:100ml:4g:4 g.
Dissolving triclopyr, diuron, deionized water and an auxiliary agent in the formula into a uniform water phase; under high-speed stirring, the mixture is prepared into the sugarcane composite suspending agent prepared from triclopyr and diuron.
Example 3:
a compound herbicide for sugarcane based on triclopyr and diuron is a dosage form wettable powder of the herbicide, and comprises the following raw materials of, by weight, 40% of triclopyr, 25% of diuron, 8% of an auxiliary agent, and the balance of a mixture of starch and light calcium carbonate in a mass ratio of 1: 1.
Wherein the auxiliary agent is a mixture of amphiphilic chitosan, sodium carboxymethylcellulose, epoxidized soybean oil and propanol in a mass ratio of 1:1:1: 1.
The preparation method of the amphiphilic chitosan comprises the following steps:
step A, dissolving chitosan in 1% acetic acid water solution, filtering insoluble substances, adding sodium hydroxide into the dissolved filtrate under stirring to obtain white precipitate, and filtering; soaking the filter cake in distilled water, adjusting the pH of the solution to 7 with hydrochloric acid, and filtering; washing with distilled water for multiple times, precipitating with acetone, filtering, and drying the filter cake in a vacuum drying oven at 50 deg.C for 1h to obtain treated chitosan; filling the treated chitosan into a reaction bottle with a stirrer, adding a sodium hydroxide solution with the mass concentration of 35% and isopropanol, stirring to react for 50min, slowly dropwise adding monochloroacetic acid, completing the dropwise adding within 30min, heating to 60 ℃, continuing to stir to react for 3h, neutralizing to be neutral by using dilute hydrochloric acid after the reaction is stopped, precipitating the product by using acetone, filtering, washing for 2 times by using an 85% methanol solution, washing for 1 time by using anhydrous methanol, precipitating by using acetone, filtering, and placing a filter cake at 30 ℃ for vacuum drying to obtain carboxymethyl chitosan, wherein the dosage ratio of the chitosan, an acetic acid aqueous solution, the sodium hydroxide and the hydrochloric acid in the step A is 15g:800ml:1 mol; the using ratio of the treated chitosan to the sodium hydroxide solution to the treated isopropanol to the treated monochloroacetic acid is 12g to 60ml to 30ml to 6 g;
b, dissolving the carboxymethyl chitosan obtained in the step A in a water-alcohol solution, stirring and swelling for 2 hours at 30 ℃, then adding phosphotungstic acid and hydrogen peroxide with the mass concentration of 30%, carrying out reflux reaction for 1 hour at 70 ℃, carrying out ultrasonic treatment for 30min, then precipitating the product by using propanol, filtering, washing for 2 times by using a methanol solution with the concentration of 85%, washing for 1 time by using anhydrous methanol, precipitating by using acetone, filtering, and carrying out vacuum drying on a filter cake at 30 ℃ to obtain the treated carboxymethyl chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4:1, and the dosage ratio of the carboxymethyl chitosan, the water-alcohol solution, the phosphotungstic acid and the hydrogen peroxide is 9g:150mL:6mg:6 mL;
and step C, putting the carboxymethyl chitosan treated in the step B into a water-alcohol solution, adding allyl glycidyl ether, uniformly stirring, reacting for 2 hours at 95 ℃, adding dodecyl trimethoxy silane, reacting for 3 hours at 70 ℃, precipitating the product with propanol, filtering, washing with 85% methanol solution for 2 times, washing with anhydrous methanol for 1 time, precipitating with acetone, filtering, and drying the filter cake in vacuum at 30 ℃ to obtain the amphiphilic chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4:1, and the dosage ratio of the carboxymethyl chitosan, the water-alcohol solution, the allyl glycidyl ether and the dodecyl trimethoxy silane after being treated in the step C is 13g:120ml:6g:6 g.
The triclopyr, diuron, diatomite and bentonite in the formula are crushed to form mixed powder, the mixed auxiliary agent is put into the mixed powder, and the wettable powder is prepared after the air flow crushing and mixing.
Example 4:
a compound herbicide based on triclopyr and diuron for sugarcane is a dispersible suspending agent and comprises the following raw materials, by weight, 20% of triclopyr, 25% of diuron, 8% of an auxiliary agent and the balance of deionized water.
Wherein the auxiliary agent is a mixture of amphiphilic chitosan, sodium carboxymethylcellulose, epoxidized soybean oil and propanol in a mass ratio of 1:1:1: 1.
The preparation method of the amphiphilic chitosan comprises the following steps:
step A, dissolving chitosan in 1% acetic acid water solution, filtering insoluble substances, adding sodium hydroxide into the dissolved filtrate under stirring to obtain white precipitate, and filtering; soaking the filter cake in distilled water, adjusting the pH of the solution to 7 with hydrochloric acid, and filtering; washing with distilled water for multiple times, precipitating with acetone, filtering, and drying the filter cake in a vacuum drying oven at 50 deg.C for 1h to obtain treated chitosan; filling the treated chitosan into a reaction bottle with a stirrer, adding a sodium hydroxide solution with the mass concentration of 35% and isopropanol, stirring to react for 50min, slowly dropwise adding monochloroacetic acid, completing the dropwise adding within 30min, heating to 60 ℃, continuing to stir to react for 3h, neutralizing to be neutral by using dilute hydrochloric acid after the reaction is stopped, precipitating the product by using acetone, filtering, washing for 2 times by using an 85% methanol solution, washing for 1 time by using anhydrous methanol, precipitating by using acetone, filtering, and placing a filter cake at 30 ℃ for vacuum drying to obtain carboxymethyl chitosan, wherein the dosage ratio of the chitosan, an acetic acid aqueous solution, the sodium hydroxide and the hydrochloric acid in the step A is 15g:800ml:1 mol; the using ratio of the treated chitosan to the sodium hydroxide solution to the treated isopropanol to the treated monochloroacetic acid is 12g to 60ml to 30ml to 6 g;
b, dissolving the carboxymethyl chitosan obtained in the step A in a water-alcohol solution, stirring and swelling for 2 hours at 30 ℃, then adding phosphotungstic acid and hydrogen peroxide with the mass concentration of 30%, carrying out reflux reaction for 1 hour at 70 ℃, carrying out ultrasonic treatment for 30min, then precipitating the product by using propanol, filtering, washing for 2 times by using a methanol solution with the concentration of 85%, washing for 1 time by using anhydrous methanol, precipitating by using acetone, filtering, and carrying out vacuum drying on a filter cake at 30 ℃ to obtain the treated carboxymethyl chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4:1, and the dosage ratio of the carboxymethyl chitosan, the water-alcohol solution, the phosphotungstic acid and the hydrogen peroxide is 9g:150mL:6mg:6 mL;
and step C, putting the carboxymethyl chitosan treated in the step B into a water-alcohol solution, adding allyl glycidyl ether, uniformly stirring, reacting for 2 hours at 95 ℃, adding dodecyl trimethoxy silane, reacting for 3 hours at 70 ℃, precipitating the product with propanol, filtering, washing with 85% methanol solution for 2 times, washing with anhydrous methanol for 1 time, precipitating with acetone, filtering, and drying the filter cake in vacuum at 30 ℃ to obtain the amphiphilic chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4:1, and the dosage ratio of the carboxymethyl chitosan, the water-alcohol solution, the allyl glycidyl ether and the dodecyl trimethoxy silane after being treated in the step C is 13g:120ml:6g:6 g.
The preparation method comprises the steps of crushing triclopyr, diuron and diatomite in the formula to form mixed powder, adding the mixed auxiliary agent into the mixed powder, adding the balance of deionized water, crushing by using a superfine jet mill, kneading, adding into a fluidized bed granulation dryer, granulating, drying and screening to obtain the triclopyr and diuron-based sugarcane composite water dispersible granule.
Comparative example 1:
a composite herbicide based on triclopyr and diuron for sugarcane is a dispersible suspending agent and comprises the following raw materials, by weight, 20% of triclopyr, 15% of diuron, 3% of an auxiliary agent and the balance of propanol.
Wherein the auxiliary agent is a mixture of carboxymethyl chitosan, sodium carboxymethyl cellulose, epoxidized soybean oil and propanol, and the mass ratio of the carboxymethyl chitosan to the sodium carboxymethyl cellulose to the propanol is 1.5:15:0.5: 0.5.
The preparation method of the carboxymethyl chitosan comprises the following steps:
step A, dissolving chitosan in 1% acetic acid water solution, filtering insoluble substances, adding sodium hydroxide into the dissolved filtrate under stirring to obtain white precipitate, and filtering; soaking the filter cake in distilled water, adjusting the pH of the solution to 7 with hydrochloric acid, and filtering; washing with distilled water for multiple times, precipitating with acetone, filtering, and drying the filter cake in a vacuum drying oven at 50 deg.C for 1h to obtain treated chitosan; filling the treated chitosan into a reaction bottle with a stirrer, adding a sodium hydroxide solution with the mass concentration of 35% and isopropanol, stirring to react for 50min, slowly dropwise adding monochloroacetic acid, completing the dropwise adding within 30min, heating to 60 ℃, continuing to stir to react for 3h, neutralizing to be neutral by using dilute hydrochloric acid after the reaction is stopped, precipitating the product by using acetone, filtering, washing for 2 times by using an 85% methanol solution, washing for 1 time by using anhydrous methanol, precipitating by using acetone, filtering, and placing a filter cake at 30 ℃ for vacuum drying to obtain carboxymethyl chitosan, wherein the dosage ratio of the chitosan, an acetic acid aqueous solution, the sodium hydroxide and the hydrochloric acid in the step A is 10g:500ml:1 mol; the using ratio of the treated chitosan to the sodium hydroxide solution to the treated isopropanol to the treated monochloroacetic acid is 5g to 30ml to 20ml to 3 g;
and step B, dissolving the carboxymethyl chitosan obtained in the step A in a water-alcohol solution, stirring and swelling for 2 hours at 30 ℃, adding phosphotungstic acid and hydrogen peroxide with the mass concentration of 30%, refluxing and reacting for 1 hour at 70 ℃, performing ultrasonic treatment for 30 minutes, precipitating and filtering a product by using propanol, washing the product for 2 times by using a methanol solution with the concentration of 85%, washing the product for 1 time by using anhydrous methanol, precipitating by using acetone, filtering, and performing vacuum drying on a filter cake at 30 ℃ to obtain the treated carboxymethyl chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4:1, and the dosage ratio of the carboxymethyl chitosan to the water-alcohol solution, the phosphotungstic acid to the hydrogen peroxide is 5g:100mL:3mg:3 mL.
Dissolving triclopyr, diuron, propanol and an auxiliary agent in the formula into a uniform oil phase; under high-speed stirring, the triclopyr and diuron are mixed to prepare the sugarcane composite dispersible suspending agent.
Comparative example 2:
a compound herbicide based on triclopyr and diuron for sugarcane is a suspending agent and comprises the following raw materials, by weight, 30% of triclopyr, 10% of diuron, 6% of an auxiliary agent and the balance of deionized water.
Wherein the auxiliary agent is chitosan, sodium carboxymethylcellulose, epoxidized soybean oil and propanol according to the mass ratio of 1:1:1: 1.
Dissolving triclopyr, diuron, deionized water and an auxiliary agent in the formula into a uniform water phase; under high-speed stirring, the mixture is prepared into the sugarcane composite suspending agent prepared from triclopyr and diuron.
Comparative example 3:
compared with the example 3, the diuron in the formula is changed into the triclopyr, and the rest steps are the same, so that the sugarcane wettable powder containing 65% of triclopyr is finally obtained.
Comparative example 4:
compared with the example 4, the triclopyr in the formula is changed into diuron, and the rest steps are the same, so that the water dispersible granule for the sugarcane containing 55% of diuron is finally obtained.
The herbicides obtained in examples 1 to 4 and comparative examples 1 to 4 were applied to 8 test sugarcane fields, and the sugarcane varieties used in the 8 test sugarcane fields were the same in other management means, and the herbicidal effects after 30 days were observed to obtain the test data shown below.
As can be seen from the above data, the herbicidal effects of examples 1 to 4 are superior to those of comparative examples 1 to 4.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely exemplary and illustrative of the principles of the present invention and various modifications, additions and substitutions of the specific embodiments described herein may be made by those skilled in the art without departing from the principles of the present invention or exceeding the scope of the claims set forth herein.
Claims (6)
1. A composite herbicide based on triclopyr and diuron for sugarcane is characterized by comprising the following raw materials, by weight, 1-60% of triclopyr, 1-30% of diuron, 3-8% of an auxiliary agent, and the balance of a carrier.
2. The compound herbicide based on triclopyr and diuron for sugarcane as claimed in claim 1, wherein the adjuvant is a mixture of amphiphilic chitosan, sodium carboxymethylcellulose, epoxidized soybean oil and propanol in any ratio.
3. The compound herbicide based on triclopyr and diuron for sugarcane according to claim 1, wherein the preparation method of the amphiphilic chitosan comprises the following steps:
step A, dissolving chitosan in 1% acetic acid water solution, filtering insoluble substances, adding sodium hydroxide into the dissolved filtrate under stirring to obtain white precipitate, and filtering; soaking the filter cake in distilled water, adjusting the pH of the solution to 6-7 with hydrochloric acid, and filtering; washing with distilled water for multiple times, precipitating with acetone, filtering, and drying the filter cake in a vacuum drying oven at 50-60 deg.C for 1h to obtain treated chitosan; filling the treated chitosan into a reaction bottle with a stirrer, adding sodium hydroxide solution with the mass concentration of 35% and isopropanol, stirring to react for 50min, slowly dropwise adding monochloroacetic acid, completing the dropwise adding within 30min, heating to 60-65 ℃, continuing to stir to react for 3h, neutralizing to be neutral by using dilute hydrochloric acid after the reaction is stopped, precipitating and filtering a product by using acetone, washing for 2-3 times by using 85% methanol solution, washing for 1 time by using anhydrous methanol, precipitating and filtering by using acetone, and placing a filter cake at 30-35 ℃ for vacuum drying to obtain carboxymethyl chitosan;
b, dissolving the carboxymethyl chitosan obtained in the step A in a water-alcohol solution, stirring and swelling for 2-3h at 30-35 ℃, adding phosphotungstic acid and hydrogen peroxide with the mass concentration of 30%, performing reflux reaction for 1-3h at 60-70 ℃, performing ultrasonic treatment for 30min, precipitating the product with propanol, filtering, washing for 2-3 times with 85% methanol solution, washing for 1 time with anhydrous methanol, precipitating with acetone, filtering, and performing vacuum drying on the filter cake at 30-35 ℃ to obtain the treated carboxymethyl chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4: 1;
and step C, putting the carboxymethyl chitosan treated in the step B into a water-alcohol solution, adding allyl glycidyl ether, uniformly stirring, reacting for 2 hours at the temperature of 80-95 ℃, adding dodecyl trimethoxy silane, reacting for 3-5 hours at the temperature of 70-80 ℃, precipitating the product with propanol, filtering, washing the product with 85% methanol solution for 2-3 times, washing with anhydrous methanol for 1 time, precipitating with acetone, filtering, and drying the filter cake in vacuum at the temperature of 30-35 ℃ to obtain the amphiphilic chitosan, wherein the volume ratio of water to anhydrous ethanol in the water-alcohol solution is 4: 1.
4. The compound herbicide based on triclopyr and diuron for sugarcane as claimed in claim 3, wherein the amount ratio of chitosan, acetic acid aqueous solution, sodium hydroxide and hydrochloric acid in step A is 10-15g: 500-; the usage ratio of the treated chitosan, the sodium hydroxide solution, the isopropanol and the monochloroacetic acid is 5-12g, 30-60ml, 20-30ml and 3-6 g.
5. The compound herbicide based on triclopyr and diuron for sugarcane as claimed in claim 3, wherein the amount ratio of carboxymethyl chitosan to hydroalcoholic solution to phosphotungstic acid to hydrogen peroxide in step B is 5g: 100-.
6. The compound herbicide based on triclopyr and diuron for sugarcane according to claim 3, wherein the amount ratio of the carboxymethyl chitosan, the hydroalcoholic solution, the allyl glycidyl ether and the dodecyl trimethoxy silane after being treated in the step C is 6-13g, 80-120ml, 3-6g and 3-6 g.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114946861A (en) * | 2022-05-28 | 2022-08-30 | 河北上瑞生物科技有限公司 | Pesticide composition containing chitosan and kasugamycin, preparation method and application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114946861A (en) * | 2022-05-28 | 2022-08-30 | 河北上瑞生物科技有限公司 | Pesticide composition containing chitosan and kasugamycin, preparation method and application |
| CN114946861B (en) * | 2022-05-28 | 2023-10-31 | 河北上瑞生物科技有限公司 | Pesticide composition containing chitosan and kasugamycin, preparation method and application |
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