CN113508815A - Weeding composition containing triclopyr and bentazone - Google Patents

Weeding composition containing triclopyr and bentazone Download PDF

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CN113508815A
CN113508815A CN202110956644.8A CN202110956644A CN113508815A CN 113508815 A CN113508815 A CN 113508815A CN 202110956644 A CN202110956644 A CN 202110956644A CN 113508815 A CN113508815 A CN 113508815A
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bentazone
reaction
triclopyr
wetting agent
liquid
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郭晓刚
常永军
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Anhui Xitian Biotechnology Co ltd
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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
    • 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
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • 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
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12—Powders or granules
    • A01N25/14—Powders or granules wettable
    • 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
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
    • 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
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/88—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms six-membered rings with three ring hetero atoms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
    • B01D29/01—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
    • B01D29/05—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements supported
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D36/00—Filter circuits or combinations of filters with other separating devices
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00—Preparation of carboxylic acid amides
    • C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines

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  • Pest Control & Pesticides (AREA)
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Abstract

The invention discloses a herbicidal composition containing triclopyr and bentazone, and relates to the technical field of herbicides, wherein the herbicidal composition comprises the following components in parts by weight: 5-30 parts of triclopyr, 3-10 parts of bentazone, 1-8 parts of an auxiliary agent and 5-12 parts of a synergistic wetting agent; according to the invention, triclopyr and bentazone are compounded, the synergistic wetting agent is added, hydrophilic aspartic acid disodium groups exist on the surface of the synergistic wetting agent, and carboxyl groups and amide groups which are the same as those of the bentazone and the triclopyr exist on the surface of the synergistic wetting agent, so that the triclopyr and the bentazone can be well compatible and foamed in an aqueous solution; the weeding composition is kept wet by a plurality of amino groups and carboxyl groups existing on the cocoyl disodium aspartate, the bentazone and the triclopyr are well diffused and slowly released to exert the effect, the dosage of the weeding composition is reduced, the weeding effective period is prolonged, the biodegradability is good, and the safety is high.

Description

Weeding composition containing triclopyr and bentazone
Technical Field
The invention relates to the technical field of herbicides, and in particular relates to a herbicidal composition containing triclopyr and bentazone.
Background
Triclopyr is an organic compound having the molecular formula C7H4O3NCl3The herbicide belongs to an internal absorption conduction type selective herbicide, is absorbed by leaf surfaces and root systems of plants, is conducted to the whole plants in the plants, causes the roots, stems and leaves of the plants to be deformed, runs out of stored substances, causes vascular bundles to be embolised or broken, causes the plants to die gradually, has drug resistance to gramineous crops, is suitable for weeding, irrigation and killing before forest forestation, maintains fire lines, supports and breeds pine trees and forest stand transformation, is used for preventing and removing broadleaf weeds and woody plants in non-cultivated lands, and can also be used for preventing and removing broadleaf weeds in fields of gramineous crops such as wheat, corn, oat, sorghum and the like;
the research reports the mixed effect of the triclopyr and penoxsulam, imazethapyr, fluroxypyr, cyhalofop-butyl, fenoxaprop-p-ethyl, propanil and molinate in the paddy field; the discovery that the mixed use of triclopyr and aryloxyphenoxypropionic acid ester herbicides such as cyhalofop-butyl, fenoxaprop-p-ethyl and the like can cause antagonistic effect and show that the control effect of the agents on gramineous weeds is reduced; the triclopyr and glufosinate can also generate antagonistic effect when being mixed, the barnyard grass in the paddy field has serious resistance to the penoxsulam, the compound application range of the triclopyr and the penoxsulam is limited, the safety of the fluroxypyr, the propanil and the gramineae to the paddy is found to be poor in production, and the compound application potential of the triclopyr and the agents is limited at present;
bentazone is a heterocyclic contact-type and slightly systemic herbicide, the action mechanism is mainly absorbed by leaves (the roots in paddy fields can also be absorbed), the bentazone permeates through the leaves and is conducted into chloroplasts, the electronic transmission of photosynthesis is inhibited, the oxidation absorption and assimilation processes in the combination process within 2 hours after the application of the herbicide are inhibited, the bentazone stops completely within 11 hours, the leaves wither and turn yellow, and finally the bentazone is dead;
at present, researchers have prepared a plurality of different herbicides, but the problems of weed drug resistance and resistance evolution and the like are easily caused by long-term continuous high-dose chemical herbicides using single varieties or single action modes, the reasonable compounding or mixing of the herbicides has the advantages of expanding the weed control spectrum, improving the control effect, delaying the drug resistance of weeds, generating and developing the drug resistance and the like, the existing compound herbicidal composition of the triclopyr and the bentazone is only reported, how to develop an auxiliary agent capable of promoting the bentazone and the triclopyr to be well compatible and foamed is important for improving the performance, reducing the dosage and toxicity of the herbicidal composition and improving the safety and the slow release effect.
Disclosure of Invention
The invention aims to provide a weeding composition containing triclopyr and bentazone, which is prepared by compounding triclopyr and bentazone, adding a synergistic wetting agent, wherein the surface of the synergistic wetting agent has hydrophilic aspartic acid disodium groups, and has the same carboxyl and amide groups as bentazone and triclopyr, and the synergistic wetting agent can be well compatible with the bentazone and the triclopyr and can be foamed in an aqueous solution; the weeding composition is kept wet by a plurality of amino groups and carboxyl groups on the disodium cocoyl aspartate, so that the bentazone and the triclopyr can be well diffused and slowly released to exert the effect, the dosage of the weeding composition is reduced, and the effective period of weeding is prolonged; the synergistic wetting agent is synthesized based on natural molecules, has good biodegradability, does not generate residual toxicity to crops, and has high safety; is used for solving the problems of improving the slow release performance of the weeding composition, reducing the dosage and toxicity, and improving the safety and control effect in the prior art.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a herbicidal composition containing triclopyr and bentazone, which comprises the following components in parts by weight: 5-30 parts of triclopyr, 3-10 parts of bentazone, 1-8 parts of an auxiliary agent and 5-12 parts of a synergistic wetting agent;
the preparation method of the synergistic wetting agent comprises the following steps:
step one, mixing aspartic acid and a sodium hydroxide solution in a reaction kettle, adding a solvent, heating to 70-80 ℃, stirring and reacting for 2-3 hours, monitoring the pH value in real time by using a pH meter in the reaction process, and adding the sodium hydroxide solution through a peristaltic pump to adjust the pH value of a reaction solution to 10-11 to obtain a disodium aspartate reaction solution;
dropwise adding coconut oil acyl chloride into the aspartic acid disodium reaction liquid through another peristaltic pump, stirring and reacting at 25-35 ℃, and simultaneously adding a sodium hydroxide solution into the reaction kettle to keep the pH value of the reaction system between 12 and 13 to obtain coconut oil acylation reaction liquid;
and step three, dripping a hydrochloric acid solution into the coconut oil acylation reaction liquid under the condition of an ice ethanol bath at the temperature of between 5 ℃ below zero and 5 ℃ until the pH is adjusted to between 9 and 10 to obtain an acidification reaction liquid, decoloring, filtering and concentrating the acidification reaction liquid to obtain a concentrated solution, carrying out vacuum freeze drying on the concentrated solution under the conditions of the pressure of between 25 and 35Pa and the temperature of between 20 ℃ below zero and 10 ℃, and then carrying out heating drying under normal pressure to obtain a pure product of the cocoyl aspartic acid disodium, namely the synergistic wetting agent.
The chemical reaction formula of the synergistic wetting agent is as follows:
Figure BDA0003220565040000031
Figure BDA0003220565040000041
the invention relates to a weeding composition containing triclopyr and bentazone, wherein the triclopyr in the ingredients is used as a systemic conduction type selective herbicide, is absorbed by leaf surfaces and root systems of plants, and is conducted to the whole plant in the plant body; bentazone is taken as a heterocyclic contact-type and slight systemic herbicide, is mainly absorbed by leaves, can be absorbed by root systems in paddy fields, and is conducted into chloroplasts through leaf surface penetration to inhibit electronic transfer of photosynthesis; however, the bentazone has the obvious characteristics of high activity and good weeding effect in a high-temperature sunny day, and is easy to be absorbed by leaves and root systems of weeds in a dry environment to exert the maximum effect, so that in order to exert the weeding effect after the bentazone and the triclopyr are compounded, a synergistic wetting auxiliary agent capable of promoting the bentazone and the triclopyr to be well compatible and foamed is needed, the slow release performance of the weeding composition is improved, and the dosage and toxicity are reduced.
The synergistic wetting auxiliary agent adopts a pure cocoyl disodium aspartate product, the surface of the synergistic wetting auxiliary agent has hydrophilic disodium aspartate groups, the water solubility of the synergistic wetting auxiliary agent is superior to that of other amino acid groups due to the existence of the two disodium aspartate groups, and meanwhile, the long carbon chain of the cocoyl group can increase the hydrophobicity, so that the synergistic wetting auxiliary agent has proper water solubility, has the same carboxyl and amide groups as bentazone and triclopyr, and can be well compatible with the bentazone and the triclopyr and foam in an aqueous solution; the weeding composition is kept wet by a plurality of amino groups and carboxyl groups on the disodium cocoyl aspartate, so that the bentazone and the triclopyr can be well diffused and slowly released to exert the effect, the dosage of the weeding composition is reduced, and the effective period of weeding is prolonged; the synergistic wetting agent is synthesized based on natural molecules, has good biodegradability, does not generate residual toxicity to crops, and has high safety.
The preparation method of the synergistic wetting agent comprises the steps of reacting aspartic acid in an alkaline environment of sodium hydroxide, monitoring the pH value in real time, and adding a sodium hydroxide solution to adjust the pH value to obtain a reaction solution of disodium aspartate; keeping the pH value of the aspartic acid disodium reaction solution under an alkaline condition, and stirring for reaction to obtain a coconut oil acylation reaction solution; acidifying, decoloring, filtering, concentrating, vacuum freeze-drying and normal-pressure heating drying the coconut oil acylation reaction liquid to obtain a pure product of the cocoyl aspartic acid disodium; the continuous reaction in the reaction kettle is matched with the real-time monitoring of pH, so that the purity and yield of the pure cocoyl aspartic acid disodium are improved.
As a further preferable scheme of the invention, in the first step, the solvent is one or a mixture of more of deionized water, cyclopentanone, cyclohexanone, N-dimethylformamide and ethyl acetate, and the amount of the solvent is 10-20 times of the mass of the aspartic acid; the concentration of the sodium hydroxide solution is 20-40 wt%; the stirring adopts mechanical stirring, and the rotating speed is 400-600 rpm.
As a further preferable scheme of the invention, the mole ratio of the coconut oil acyl chloride to the aspartic acid in the second step is 0.95-1.2: 1, the concentration of the sodium hydroxide solution is 25 wt% to 50 wt%.
As a further preferable scheme of the invention, the concentration of the hydrochloric acid solution in the step three is 18 wt% to 35 wt%; the vacuum freeze drying process of the concentrated solution under the conditions of the pressure of 25-35Pa and the temperature of-20 to-10 ℃ is as follows: freezing at-15- -10 deg.C under 30-35Pa for 2-4 hr, and freezing at-20- -15 deg.C under 15-30Pa for 3-5 hr; the normal pressure heating drying is to be specific, drying is carried out for 4-6 hours at the temperature of 55-65 ℃.
As a further preferable scheme of the invention, the pesticide formulation prepared by the weeding composition is one of suspoemulsion, water suspending agent, dispersible oil suspending agent, missible oil, wettable powder, water dispersible granule and emulsion in water.
As a further preferable embodiment of the present invention, the auxiliary agent is selected from one or more of organic bentonite, white carbon black, diatomite, and sodium dodecyl sulfate.
As a further preferable scheme of the invention, the synergistic wetting agent processing device comprises a reaction kettle, a jacket is arranged on the inner layer of the reaction kettle, the inner cavity of the reaction kettle comprises a reaction cavity, a decoloring cavity, a filtering cavity and a liquid storage cavity which are sequentially arranged from top to bottom, a speed reduction motor is arranged at the top of the reaction kettle, the speed reduction motor is connected with a stirring shaft extending into the reaction cavity through a coupling, and stirring blades are arranged at the bottom of the stirring shaft; the one side top of reation kettle is equipped with the pH meter that stretches into the reaction intracavity, and the opposite side is equipped with the flange that stretches into the reaction intracavity, is equipped with first feed liquor hole and second feed liquor hole on the flange, and first feed liquor hole has first peristaltic pump through first feed liquor union coupling, and second feed liquor hole has the second peristaltic pump through second feed liquor union coupling.
As a further preferable scheme of the invention, the bottom of the reaction cavity is provided with a liquid baffle, the central bottom of the liquid baffle is provided with a discharge valve, the bottom of the decoloring cavity is provided with a decoloring plate, and the decoloring plate is filled with a decoloring agent; a filter plate is arranged at the bottom of the filter cavity, and filter cloth is placed on the filter plate; the bottom in stock solution chamber is connected with concentrated jar through the fluid-discharge tube, is equipped with the elevator pump on the route of fluid-discharge tube, and the top of concentrated jar is connected with the vacuum pump through the vacuum tube.
The invention has the following beneficial effects:
1. the weeding composition is prepared by compounding triclopyr and bentazone, adding the synergistic wetting agent, wherein hydrophilic aspartic acid disodium groups exist on the surface of the synergistic wetting agent, and carboxyl groups and amide groups which are the same as those of the bentazone and the triclopyr exist, so that the triclopyr and the bentazone can be well compatible and foamed in an aqueous solution; the weeding composition is kept wet by a plurality of amino groups and carboxyl groups on the disodium cocoyl aspartate, so that the bentazone and the triclopyr can be well diffused and slowly released to exert the effect, the dosage of the weeding composition is reduced, and the effective period of weeding is prolonged; the synergistic wetting agent is synthesized based on natural molecules, has good biodegradability, does not generate residual toxicity to crops, and has high safety;
2. processingequipment of increase wetting agent, connect two peristaltic pumps through flange, make this reation kettle in reaction process, add sodium hydroxide solution when synthesizing disodium aspartate reaction liquid through first peristaltic pump, add coconut oil acyl chloride when synthesizing coconut oil acylation reaction liquid through the second peristaltic pump, make things convenient for the interpolation of reaction raw materials, the reaction chamber that simultaneously from the top down sets gradually, the decoloration chamber, filter chamber and stock solution chamber, hydrochloric acid solution adjusts behind the pH, accomplish the decoloration of reaction liquid in reation kettle, filtering process, avoid the loss that produces in the reaction liquid transfer process, improve the productivity of increase wetting agent.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an apparatus for processing an enhanced wetting agent according to an embodiment of the present invention;
FIG. 2 is a top view of a coupling flange according to an embodiment of the present invention;
FIG. 3 is a top view of a decolorizing plate in an embodiment of the present invention;
FIG. 4 is a top view of a filter plate according to an embodiment of the present invention.
Reference numerals: 100. a reaction kettle; 110. a jacket; 120. a reaction chamber; 121. a liquid baffle; 122. a discharge valve; 130. a decolorizing chamber; 131. a decolorizing plate; 140. a filter chamber; 141. a filter plate; 142. filtering cloth; 150. a liquid storage cavity; 160. a reduction motor; 161. a coupling; 162. a stirring shaft; 163. a stirring blade; 170. a pH meter; 180. a connecting flange; 181. a first liquid inlet hole; 182. a second liquid inlet hole; 183. a first liquid inlet pipe; 184. a first peristaltic pump; 185. a second liquid inlet pipe; 186. a second peristaltic pump; 190. a liquid discharge pipe; 191. a lift pump; 200. a concentration tank; 210. a vacuum tube; 220. a vacuum pump.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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:
the embodiment provides a herbicidal composition containing triclopyr and bentazone, which comprises the following components in parts by weight: 25 parts of triclopyr, 7 parts of bentazone, 5 parts of an auxiliary agent and 10 parts of a synergistic wetting agent; wherein the auxiliary agent is selected from organic bentonite.
The preparation method of the synergistic wetting agent comprises the following steps:
step one, after 133.1g (1mol) of aspartic acid and 25 wt% of sodium hydroxide solution are mixed in a reaction kettle, 1996.5g of solvent deionized water is added, the temperature is raised to 75 ℃, the mixture is stirred at a rotation speed of 550rpm and reacts for 2.6 hours, a pH meter is used for monitoring the pH value in real time in the reaction process, and the sodium hydroxide solution is added through a peristaltic pump to adjust the pH value of the reaction liquid to 10.6, so that a disodium aspartate reaction liquid is obtained;
step two, dripping 281.18g (0.98mol) of coconut oil acyl chloride into the aspartic acid disodium reaction liquid through another peristaltic pump, stirring for reaction at 32 ℃, and simultaneously adding 40 wt% of sodium hydroxide solution into the reaction kettle to keep the pH value of the reaction system between 12 and 13 to obtain coconut oil acylation reaction liquid;
step three, dripping 25 wt% hydrochloric acid solution into the coconut oil acylation reaction liquid under the condition of 3 ℃ of an ice-ethanol bath until the pH is adjusted to 9.5 to obtain an acidification reaction liquid, decoloring, filtering and concentrating the acidification reaction liquid to obtain a concentrated solution, freezing the concentrated solution for 3.5 hours under the conditions of pressure of 32Pa and temperature of-12 ℃, and then freezing for 4 hours under the conditions of pressure of 22Pa and temperature of-17 ℃; and then drying at the temperature of 62 ℃ for 5.5 hours to obtain the pure product of the cocoyl aspartic acid disodium, namely the synergistic wetting agent, wherein the detection yield reaches 91.5%, and the purity reaches 98.5%.
Example 2:
the embodiment provides a herbicidal composition containing triclopyr and bentazone, which comprises the following components in parts by weight: 16 parts of triclopyr, 7 parts of bentazone, 3 parts of an auxiliary agent and 7 parts of a synergistic wetting agent; wherein the auxiliary agent is selected from diatomite.
The preparation method of the synergistic wetting agent comprises the following steps:
step one, after 133.1g (1mol) of aspartic acid and 32 wt% of sodium hydroxide solution are mixed in a reaction kettle, 2395.8g of solvent cyclohexanone is added, the temperature is raised to 78 ℃, the mixture is stirred at 480rpm and reacts for 2.2 hours, a pH meter is used for monitoring the pH in real time during the reaction process, the sodium hydroxide solution is added through a peristaltic pump to adjust the pH value of the reaction solution to 10.2, and a disodium aspartate reaction solution is obtained;
step two, dripping 315.61g (1.1mol) of coconut oil acyl chloride into the aspartic acid disodium reaction liquid through another peristaltic pump, stirring for reaction at 35 ℃, and simultaneously adding 46 wt% of sodium hydroxide solution into the reaction kettle to keep the pH value of the reaction system between 12 and 13 to obtain coconut oil acylation reaction liquid;
step three, dripping 30 wt% hydrochloric acid solution into the coconut oil acylation reaction liquid under the condition of an ice-ethanol bath at the temperature of-5 ℃ until the pH is adjusted to 9.8 to obtain an acidification reaction liquid, decoloring, filtering and concentrating the acidification reaction liquid to obtain a concentrated solution, freezing the concentrated solution for 3.2 hours under the conditions of the pressure of 28Pa and the temperature of-16 ℃, and then freezing for 4 hours under the conditions of the pressure of 20Pa and the temperature of-18 ℃; and then drying at the temperature of 60 ℃ for 4.8 hours to obtain the pure product of the cocoyl aspartic acid disodium, namely the synergistic wetting agent, wherein the detection yield reaches 90.9 percent, and the purity reaches 98.8 percent.
Example 3:
the embodiment provides a herbicidal composition containing triclopyr and bentazone, which comprises the following components in parts by weight: 22 parts of triclopyr, 6 parts of bentazone, 5 parts of an auxiliary agent and 8 parts of a synergistic wetting agent; the auxiliary agent is selected from sodium dodecyl sulfate.
The preparation method of the synergistic wetting agent comprises the following steps:
step one, after 133.1g (1mol) of aspartic acid and 25 wt% of sodium hydroxide solution are mixed in a reaction kettle, 2129.6g of solvent N, N-dimethylformamide is added, the temperature is raised to 76 ℃, the reaction is stirred at 580rpm for 2.3 hours, a pH meter is used for monitoring the pH in real time during the reaction process, the sodium hydroxide solution is added through a peristaltic pump to adjust the pH value of the reaction solution to 10.8, and the aspartic acid disodium reaction solution is obtained;
step two, dripping 344.3g (1.2mol) of coconut oil acyl chloride into the aspartic acid disodium reaction liquid through another peristaltic pump, stirring for reaction at 30 ℃, and simultaneously adding 46 wt% of sodium hydroxide solution into the reaction kettle to keep the pH value of the reaction system between 12 and 13 to obtain coconut oil acylation reaction liquid;
step three, dripping 32 wt% hydrochloric acid solution into the coconut oil acylation reaction liquid under the condition of an ice-ethanol bath at the temperature of-5 ℃ until the pH is adjusted to 9-10 to obtain an acidification reaction liquid, decoloring, filtering and concentrating the acidification reaction liquid to obtain a concentrated solution, freezing the concentrated solution for 3.6 hours under the conditions of the pressure of 30Pa and the temperature of-18 ℃, and then freezing for 4.5 hours under the conditions of the pressure of 28Pa and the temperature of-18 ℃; and then drying for 6 hours at the temperature of 60 ℃ to obtain the pure product of the cocoyl aspartic acid disodium, namely the synergistic wetting agent, wherein the detection yield reaches 91.2%, and the purity reaches 98.7%.
Example 4:
as shown in fig. 1 to 4, the present embodiment provides a processing apparatus for synergistic wetting agent, which is suitable for preparing synergistic wetting agent in embodiments 1 to 3, and includes a reaction kettle 100, an inner layer of the reaction kettle 100 is provided with a jacket 110, an inner cavity of the reaction kettle 100 includes a reaction chamber 120, a decoloring chamber 130, a filter chamber 140, and a liquid storage chamber 150, which are sequentially arranged from top to bottom, a speed reduction motor 160 is arranged at the top of the reaction kettle 100, the speed reduction motor 160 is connected to a stirring shaft 162 extending into the reaction chamber 120 through a coupling 161, and a stirring blade 163 is arranged at the bottom of the stirring shaft 162; the top of one side of the reaction kettle 100 is provided with a pH meter 170 extending into the reaction chamber 120, the other side is provided with a connecting flange 180 extending into the reaction chamber 120, the connecting flange 180 is provided with a first liquid inlet hole 181 and a second liquid inlet hole 182, the first liquid inlet hole 181 is connected with a first peristaltic pump 184 through a first liquid inlet pipe 183, and the second liquid inlet hole 182 is connected with a second peristaltic pump 186 through a second liquid inlet pipe 185.
In the processing device of the synergistic wetting agent, the speed reducing motor 160 is selected from a gear speed reducing motor with the model of R47, and the pH meter 170 is selected from an online pH meter with the model of MIK-PH 8.0; the first peristaltic pump 184 and the second peristaltic pump 186 are selected from large-flow batch type peristaltic pumps with models JS350& KZ48, the rotating speed range is 30-350rpm, and the flow range is 1.5-40L/min. Connect two peristaltic pumps through flange 180 for this reation kettle 100 is in reaction process, add sodium hydroxide solution when synthesizing disodium aspartate reaction solution through first peristaltic pump 184, add coconut oil acyl chloride when synthesizing coconut oil acylation reaction liquid through second peristaltic pump 186, make things convenient for the interpolation of reaction raw materials, reaction chamber 120 that simultaneously from the top down set gradually, decoloration chamber 130, filter chamber 140 and stock solution chamber 150, hydrochloric acid solution adjusts behind the pH, accomplish the decoloration of reaction liquid in reation kettle 100, the filtration process, avoid the loss that the reaction liquid shifts the in-process and produce.
A liquid baffle plate 121 is arranged at the bottom of the reaction chamber 120, a discharge valve 122 is arranged at the central bottom of the liquid baffle plate 121, a decolorizing plate 131 is arranged at the bottom of the decolorizing chamber 130, and a decolorizing agent is filled in the decolorizing plate 131 and is selected from activated carbon, silica gel or alumina; the bottom of the filter cavity 140 is provided with a filter plate 141, filter cloth 142 is arranged on the filter plate 141, and the aperture of the filter cloth 142 is 20-30 meshes; the bottom of the liquid storage cavity 150 is connected with a concentration tank 200 through a liquid discharge pipe 190, a lift pump 191 is arranged on the path of the liquid discharge pipe 190, and the top of the concentration tank 200 is connected with a vacuum pump 220 through a vacuum pipe 210. After the lift pump 191 is started, the filtrate formed after filtration enters the concentration tank 200 through the liquid discharge pipe 190, the vacuum pump 220 is started to suck vacuum to the concentration tank 200 through the vacuum pipe 210, and the filtrate is subjected to reduced pressure concentration to obtain a concentrated solution. The concentrated solution is further subjected to vacuum freeze drying and normal pressure heating drying to obtain the pure product of the cocoyl aspartic acid disodium.
In the processing device of the synergistic wetting agent, in the reaction process of the reaction kettle 100, a sodium hydroxide solution is added through the first peristaltic pump 184 when a disodium aspartate reaction solution is synthesized, coconut oil acyl chloride is added through the second peristaltic pump 186 when a coconut oil acylation reaction solution is synthesized, so that the addition of reaction raw materials is facilitated, meanwhile, the reaction cavity 120, the decolorizing cavity 130, the filter cavity 140 and the liquid storage cavity 150 are sequentially arranged from top to bottom, after the pH value of a hydrochloric acid solution is adjusted, the reaction kettle 100 is decolorized through a decolorizing agent in the decolorizing plate 131, and is filtered through the filter cloth 142 on the filter plate 141, so that the decolorizing and filtering processes are completed, a filtrate formed after filtering enters the concentration tank 200 through the liquid discharge pipe 190, after the vacuum pump 220 is started, the vacuum is sucked to the concentration tank 200 through the vacuum pipe 210, and the filtrate is subjected to reduced pressure concentration to obtain a concentrated solution; and (4) carrying out vacuum freeze drying and normal-pressure heating drying on the concentrated solution to obtain a pure product of the cocoyl aspartic acid disodium.
Comparative example 1:
this comparative example differs from example 1 in that no synergistic wetting agent was added.
Comparative example 2:
this comparative example differs from example 1 in that triclopyr is not added.
Comparative example 3:
this comparative example differs from example 1 in that bentazone was not added.
Comparative example 4:
this comparative example uses the compound herbicide of the examples in the patent with application No. CN202010268697.6 entitled "a compound herbicide containing triclopyr and bispyribac-sodium and its uses".
Test example:
the test method comprises the following steps: after wheat is sowed, the grass seeds to be tested are uniformly sowed on the soil surface after germination acceleration, 0.6-0.7cm of soil is covered, the grass seeds are divided into an example 1-3 group and a comparative example 1-4 group, and the field area of each group is 2m by 2 m; when the tested weeds grow to 3-5 leaf stage and 4 leaf stage of wheat, the weeding compositions prepared in examples 1-3 and comparative examples 1-4 are respectively prepared into herbicide formulations, stem and leaf spraying treatment is carried out, the dosage is controlled to be 500-600ga.i./ha, and the tested weeds are selected from gramineae weed wild oat, physalis pubescens, broadleaf weed-sowing descurainia and husbandry; the control effect of the strains after 30 days of the test is calculated, and the specific results are shown in the following table:
Figure BDA0003220565040000131
as can be seen from the above table, the herbicidal composition containing triclopyr, bentazone and a synergistic wetting agent prepared in the embodiment of the invention has good plant control effect on oat weeds, alopecurus maytans, descurainia sophia and husbandry in wheat fields, and compared with comparative examples 2-3, the combined control effect cannot be achieved by singly using the active ingredients of triclopyr or bentazone, and compared with comparative example 1, the slow release performance of the herbicidal composition cannot be improved, the dosage is reduced, and the control effect is increased without adding the synergistic wetting agent; the herbicidal composition containing triclopyr and bentazone has good control effect on gramineous weeds and broadleaf weeds, has high safety on crops, and is suitable for popularization and use.
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 preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise forms disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (8)

1. A weeding composition containing triclopyr and bentazone is characterized by comprising the following components in parts by weight: 5-30 parts of triclopyr, 3-10 parts of bentazone, 1-8 parts of an auxiliary agent and 5-12 parts of a synergistic wetting agent;
the preparation method of the synergistic wetting agent comprises the following steps:
step one, mixing aspartic acid and a sodium hydroxide solution in a reaction kettle of a synergistic wetting agent processing device, adding a solvent, heating to 70-80 ℃, stirring and reacting for 2-3 hours, monitoring the pH value in real time by using a pH meter in the reaction process, and adding the sodium hydroxide solution through a peristaltic pump to adjust the pH value of the reaction solution to 10-11 to obtain a disodium aspartate reaction solution;
dropwise adding coconut oil acyl chloride into the aspartic acid disodium reaction liquid through another peristaltic pump, stirring and reacting at 25-35 ℃, and simultaneously adding a sodium hydroxide solution into the reaction kettle to keep the pH value of the reaction system between 12 and 13 to obtain coconut oil acylation reaction liquid;
and step three, dripping a hydrochloric acid solution into the coconut oil acylation reaction liquid under the condition of an ice ethanol bath at the temperature of between 5 ℃ below zero and 5 ℃ until the pH is adjusted to between 9 and 10 to obtain an acidification reaction liquid, decoloring, filtering and concentrating the acidification reaction liquid to obtain a concentrated solution, carrying out vacuum freeze drying on the concentrated solution under the conditions of the pressure of between 25 and 35Pa and the temperature of between 20 ℃ below zero and 10 ℃, and then carrying out heating drying under normal pressure to obtain a pure product of the cocoyl aspartic acid disodium, namely the synergistic wetting agent.
2. The herbicidal composition containing triclopyr and bentazone as claimed in claim 1, wherein the solvent in step one is selected from the group consisting of deionized water, cyclopentanone, cyclohexanone, N-dimethylformamide, ethyl acetate, in an amount of 10-20 times the mass of aspartic acid; the concentration of the sodium hydroxide solution is 20-40 wt%; the stirring adopts mechanical stirring, and the rotating speed is 400-600 rpm.
3. The herbicidal composition as claimed in claim 1, wherein the molar ratio of cocoyl chloride to aspartic acid in step two is 0.95-1.2: 1, the concentration of the sodium hydroxide solution is 25 wt% to 50 wt%.
4. The herbicidal composition containing triclopyr and bentazone as claimed in claim 1 wherein the concentration of the hydrochloric acid solution in step three is from 18 wt% to 35 wt%; the vacuum freeze drying process of the concentrated solution under the conditions of the pressure of 25-35Pa and the temperature of-20 to-10 ℃ is as follows: freezing at-15- -10 deg.C under 30-35Pa for 2-4 hr, and freezing at-20- -15 deg.C under 15-30Pa for 3-5 hr; the normal pressure heating drying is to be specific, drying is carried out for 4-6 hours at the temperature of 55-65 ℃.
5. The herbicidal composition containing triclopyr and bentazone as claimed in claim 1, wherein the herbicidal composition is formulated in the form of one of a suspoemulsion, a water suspension, a dispersible oil suspension, an emulsifiable concentrate, a wettable powder, a water dispersible granule, and an aqueous emulsion.
6. The herbicidal composition containing triclopyr and bentazone as claimed in claim 1, wherein said adjuvant is selected from the group consisting of one or more of organobentonite, silica, diatomaceous earth and sodium dodecylsulphonate.
7. The herbicidal composition containing triclopyr and bentazone according to claim 1, wherein the synergistic wetting agent processing device comprises a reaction kettle (100), the inner layer of the reaction kettle (100) is provided with a jacket (110), the inner cavity of the reaction kettle (100) comprises a reaction chamber (120), a decolorization chamber (130), a filter chamber (140) and a liquid storage chamber (150) which are sequentially arranged from top to bottom, the top of the reaction kettle (100) is provided with a speed reduction motor (160), the speed reduction motor (160) is connected with a stirring shaft (162) extending into the reaction chamber (120) through a coupler (161), and the bottom of the stirring shaft (162) is provided with stirring blades (163); one side top of reation kettle (100) is equipped with pH meter (170) that stretch into in reaction chamber (120), and the opposite side is equipped with flange (180) that stretch into in reaction chamber (120), is equipped with first feed liquor hole (181) and second feed liquor hole (182) on flange (180), and first feed liquor hole (181) are connected with first peristaltic pump (184) through first feed liquor pipe (183), and second feed liquor hole (182) are connected with second peristaltic pump (186) through second feed liquor pipe (185).
8. The herbicidal composition containing triclopyr and bentazone as claimed in claim 7, wherein the bottom of the reaction chamber (120) is provided with a liquid baffle (121), the central bottom of the liquid baffle (121) is provided with a discharge valve (122), the bottom of the decolorizing chamber (130) is provided with a decolorizing plate (131), and the decolorizing plate (131) is filled with a decolorizing agent; a filter plate (141) is arranged at the bottom of the filter cavity (140), and filter cloth (142) is placed on the filter plate (141); the bottom of the liquid storage cavity (150) is connected with a concentration tank (200) through a liquid discharge pipe (190), a lifting pump (191) is arranged on the path of the liquid discharge pipe (190), and the top of the concentration tank (200) is connected with a vacuum pump (220) through a vacuum pipe (210).
CN202110956644.8A 2021-08-19 2021-08-19 Weeding composition containing triclopyr and bentazone Pending CN113508815A (en)

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