CN111758728A - Compound herbicide containing dicamba and preparation method thereof - Google Patents

Compound herbicide containing dicamba and preparation method thereof Download PDF

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Publication number
CN111758728A
CN111758728A CN202010709727.2A CN202010709727A CN111758728A CN 111758728 A CN111758728 A CN 111758728A CN 202010709727 A CN202010709727 A CN 202010709727A CN 111758728 A CN111758728 A CN 111758728A
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dicamba
sodium
containing compound
compound herbicide
acid
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Inventor
李明
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Zhenjiang Pioneer Cropscience Co ltd
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Zhenjiang Pioneer Cropscience Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/36Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
    • A01N37/38Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
    • A01N37/40Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic ring system
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, 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
    • A01N47/08Biocides, 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
    • A01N47/28Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/36Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof

Abstract

The invention discloses a compound herbicide containing dicamba, which comprises a first effective component and a second effective component, wherein the first effective component is the dicamba and accounts for 40-60% of the mass percentage; the second active ingredient is one or a mixture of nicosulfuron and rimsulfuron, the mass percent of the nicosulfuron is 0-15%, and the mass percent of the rimsulfuron is 0-15%; the adhesive also comprises 1-4% of wetting agent, 1-15% of dispersing agent, 0-10% of acid-base regulator, 0-5% of binder and the balance of filler. The herbicide provided by the invention is prepared by compounding dicamba and one or two of nicosulfuron and rimsulfuron according to different proportions, so that the weeding spectrum is expanded, the weeding effect is obviously improved, and the possibility of phytotoxicity on current crops and residual toxicity on succeeding crops is avoided.

Description

Compound herbicide containing dicamba and preparation method thereof
Technical Field
The invention relates to a compound herbicide containing dicamba and a preparation method thereof, belonging to the technical field of pesticides.
Background
In recent years, the development direction of pesticides reflects high efficiency, low toxicity, low residue and no pollution, and the specific expression is high safety, high biological activity and high selectivity, so that the performance of the pesticide product needs to be continuously optimized to meet the requirements of high efficiency, low toxicity and no pollution. The development of compound mixed pesticides is the current preferred and effective way, and pesticides with complementary performances can obtain the best synergistic effect by adjusting the mixture ratio of different pesticides.
Dicamba (also known as dichlord) belongs to benzoic acid series herbicides, has a systemic conduction effect, and has a remarkable control effect on annual and perennial broadleaf weeds. Is safe to gramineous plants such as corn, and can be used for preventing and killing Botrytis cinerea, Fagopyrum esculentum Moench, Chenopodium album, Stellaria mediae, Descurainia sophia, Xanthium sibiricum, Boea pellucida, Convolvulus arvensis, Equisetum arvense, and Cyprinus carpioides; after the spraying is carried out after the seedling, the medicament can be quickly absorbed by the leaves, stems and roots of the weeds, is conducted upwards and downwards through phloem, is mostly concentrated on meristems and parts with vigorous metabolic activity, and blocks the normal activity of the phytohormone, so that the phytohormone can die. After being absorbed by gramineous plants, the gramineous plants can be rapidly metabolized and decomposed to lose efficacy, and show strong drug resistance, so that the gramineous plants are safe to wheat, corn, rice and other gramineous plants. After the herbicide is applied to soil, the herbicide is decomposed by microorganisms, and the broad-leaved weeds generally have malformed curly symptoms within 24 hours and die in 15-20 days. Dicamba is commonly used for controlling annual and perennial broadleaf weeds in crop fields such as asparagus, corn, sorghum, wheat, sugarcane and the like, and also for controlling woody shrubs in farming areas.
Because the dicamba original drug has poor solubility, the dicamba salt is usually solved by a salt forming method, and the dicamba salt usually comprises dimethylamine salt and sodium salt; in the aspect of dosage forms, main dosage form products of the dicamba salt are water-soluble powder, water-soluble granules and water aqua, the common water-soluble granules in the market at present are prepared by reacting a dicamba technical material with liquid alkali, and drying after the reaction is finished to obtain the dicamba sodium salt technical material. The production method needs to be completed through two steps of sodium salt synthesis and granulation, has the problem of complex process, has high requirements on equipment, and has low raw material conversion rate, thus causing overhigh production cost.
At present, the herbicide for corn fields is limited by the safety of crops, the weed control spectrum is limited, the occurrence of weeds in the corn fields cannot be completely and effectively controlled by singly using a single herbicide, and residual toxicity to current season crops or aftercrops is easily caused by the fact that some herbicides are large in water solubility, too long in field lasting period, too large in dosage or uneven in application.
Disclosure of Invention
The purpose is as follows: in order to overcome the defects in the prior art, the invention provides the compounded herbicide containing the dicamba, the dicamba and the nicosulfuron and/or the rimsulfuron are compounded according to different proportions, the weed control spectrum is expanded, the weeding effect is obviously improved, and the possibility of generating phytotoxicity to crops in the same season and generating residual toxicity to crops in later crops is also avoided.
The technical scheme is as follows: in order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a compound herbicide containing dicamba comprises a first effective component and a second effective component, wherein the first effective component is the dicamba and accounts for 40-60% of the mass percentage; the second active ingredient is one or a mixture of nicosulfuron and rimsulfuron, the mass percent of the nicosulfuron is 0-15%, and the mass percent of the rimsulfuron is 0-15%.
Further, the paint also comprises 1-4% of wetting agent, 1-15% of dispersing agent, 0-10% of acid-base regulator, 0-5% of binder and the balance of filler by mass percentage.
Further, the wetting agent is one or a combination of several of sodium dodecyl sulfate, sodium sulfosuccinate, alkyl succinic acid sulfonate, fatty alcohol-polyoxyethylene ether, sodium alkyl benzene sulfonate and alkyl naphthalene sulfonate.
Further, the dispersing agent is one or a combination of several of alkylphenol polyoxyethylene ether formaldehyde condensate, lignosulfonate, polycarboxylate, naphthalenesulfonate formaldehyde condensate and p-methoxy fatty amido benzene sulfonic acid.
Further, the pH regulator is one or more of ethylenediamine tetraacetic acid, disodium ethylenediamine tetraacetic acid, sodium tripolyphosphate and citric acid.
Further, the binder is one or a combination of more of urea, glucose, soft white sugar, polyethylene glycol, soluble starch and sodium carboxymethylcellulose.
Further, the filler is one or a combination of more of sodium sulfate, ammonium sulfate, corn starch, kaolin, light calcium carbonate, talcum powder, wollastonite powder, sodium acetate, potassium chloride, sodium chloride and diatomite.
A preparation method of a compound herbicide containing dicamba comprises the following steps:
synthesis of dicamba sodium salt: weighing dicamba active compound and sodium carbonate according to a ratio, putting the dicamba active compound and the sodium carbonate into a trough type kneader, adding water after uniformly stirring, continuing kneading, carrying out rotary extrusion granulation after placing for a period of time, and bagging and placing for later use after the granulation is finished;
preparing materials according to a given proportion: weighing the materials according to the following mass percentage, and uniformly mixing for later use; 0-15% of nicosulfuron, 0-15% of rimsulfuron, 1-4% of a wetting agent, 1-15% of a dispersing agent, 0-10% of an acid-base regulator, 0-5% of a binder and the balance of a filler to 100%;
airflow crushing: crushing the mixed materials in a jet mill to ensure that the particle fineness meets the requirement of wet screening, and crushing for later use; the air inlet pressure and the feeding speed are controlled in the air flow crushing process, so that large fluctuation is avoided;
and (3) granulation: adding the powder subjected to jet milling into a kneader, uniformly stirring, adding a dicamba sodium salt wet material with the mass percentage of 40-60%, continuously uniformly stirring, adding water, kneading for about 5min, starting granulation, continuously and uniformly adding the wet material into a rotary extrusion granulator, controlling the feeding speed and the material level in the granulator, and keeping for later use after extrusion;
drying: starting the boiling dryer, preheating to 50 ℃, adding the materials, setting the drying temperature to 65 ℃, and performing screening detection after drying.
Further, the mass ratio of the dicamba technical material to the sodium carbonate is adjusted according to the acid strength of the dicamba technical material, and the pH value of the dicamba sodium salt is controlled to be 7.9-9.0.
Has the advantages that: compared with the prior art, the invention has the following advantages:
(1) the herbicide provided by the invention is prepared by compounding dicamba and one or two of nicosulfuron and rimsulfuron according to different proportions, so that the weeding spectrum is expanded, the weeding effect is obviously improved, and the possibility of phytotoxicity on current crops and residual toxicity on succeeding crops is avoided;
(2) according to the preparation method of the herbicide, disclosed by the invention, the dicamba original drug and the sodium carbonate are mixed at normal pressure and at the temperature of 45-55 ℃ to carry out acid-base reaction, the pH is controlled to be 7.9-9.0, the reaction is mild, the dicamba salifying reaction, kneading and granulation are carried out simultaneously, the process flow is short, the operability is strong, the raw material conversion rate is high, and the cost is obviously reduced.
Detailed Description
The present invention will be further described with reference to the following examples.
The compound herbicide containing dicamba comprises a first effective component dicamba in a mass percentage of 40-60%, a second effective component nicosulfuron and rimsulfuron in a mass percentage of 0-15%, or a mixture of nicosulfuron and rimsulfuron in a mass percentage of 0-15%; the paint also comprises 1-4% of wetting agent, 1-15% of dispersing agent, 0-10% of acid-base regulator, 0-5% of binder and the balance of filler.
The wetting agent is one or a combination of several of sodium dodecyl sulfate, sodium sulfosuccinate, alkyl succinic acid sulfonate, fatty alcohol-polyoxyethylene ether, sodium alkyl benzene sulfonate and alkyl naphthalene sulfonate.
The dispersing agent is one or a combination of more of alkylphenol polyoxyethylene ether formaldehyde condensate, lignosulfonate, polycarboxylate, alkyl naphthalene sulfonate polycondensate and p-methoxy fatty amido benzene sulfonic acid.
The pH regulator is one or more of ethylenediamine tetraacetic acid, disodium ethylenediamine tetraacetic acid, sodium tripolyphosphate and citric acid.
The binder is one or a combination of more of urea, glucose, polyethylene glycol, soluble starch and sodium carboxymethyl cellulose.
The filler is one or a combination of more of sodium sulfate, ammonium sulfate, corn starch, kaolin, light calcium carbonate, talcum powder, wollastonite powder, sodium acetate, potassium chloride, sodium chloride and diatomite.
First, preparation of reagent
Example 1: the herbicide contains 55% of dicamba, 9.2% of nicosulfuron and 2.3% of rimsulfuron
The preparation method comprises the following steps:
(1) synthesis of dicamba sodium salt
Putting 120kg of dicamba technical material and 35.2kg of sodium carbonate into a trough type kneader, adding 1.2kg of water after uniformly stirring, continuously kneading, carrying out rotary extrusion granulation after standing for about 60min, bagging after the granulation is finished, and standing for later use;
wherein the addition amount of the sodium carbonate is properly increased or decreased along with the change of the acidity of the dicamba technical product, and the pH value of the dicamba sodium salt is controlled to be between 7.0 and 9.0.
(2) Ingredients
The samples were weighed according to the following compounding schedule:
Figure DEST_PATH_IMAGE002
accurately weighing the above materials (except dicamba sodium salt), and mixing well for later use.
(3) Jet milling
Crushing the material mixed in the step (2) in a jet mill to ensure that the particle fineness meets a wet sieve (the particle size is 325 meshes), and controlling the air inlet pressure, the feeding speed and the like in the jet milling process to avoid large fluctuation; and placing the material after jet milling for later use.
(4) Granulating
Adding the powder subjected to jet milling into a kneader, uniformly stirring, adding the dicamba sodium salt wet material in proportion, continuously uniformly stirring, calculating the water addition amount according to the experimental data of a laboratory test, kneading for about 5min, starting granulation, continuously and uniformly adding the wet material into a rotary extrusion granulator, controlling the feeding speed and the material level in the granulator, and keeping for later use after the extrusion is finished.
(5) Drying by baking
Starting a boiling dryer for preheating, adding materials when the temperature reaches 50 ℃, starting drying, setting the drying temperature to be 65 ℃, and screening and detecting after drying is finished.
Example 2: the herbicide contains 40% of dicamba, 8% of nicosulfuron and 2% of rimsulfuron
The preparation method comprises the following steps:
(1) synthesis of dicamba sodium salt
Putting 120kg of dicamba technical material and 35.2kg of sodium carbonate into a trough type kneader, adding 1.2kg of water after uniformly stirring, continuously kneading, carrying out rotary extrusion granulation after standing for about 60min, bagging after the granulation is finished, and standing for later use;
wherein the addition amount of the sodium carbonate is properly increased or decreased along with the change of the acidity of the dicamba technical product, and the pH value of the dicamba sodium salt is controlled to be between 7.0 and 9.0.
(2) Ingredients
The samples were weighed according to the following compounding schedule:
Figure DEST_PATH_IMAGE004
accurately weighing the above materials (except dicamba sodium salt), and mixing well for later use.
The other steps are the same as in example 1.
Example 3: the herbicide contains 60% of dicamba and 15% of nicosulfuron
The preparation method comprises the following steps:
(1) synthesis of dicamba sodium salt
Putting 120kg of dicamba technical material and 35.2kg of sodium carbonate into a trough type kneader, adding 1.2kg of water after uniformly stirring, continuously kneading, carrying out rotary extrusion granulation after standing for about 60min, bagging after the granulation is finished, and standing for later use;
wherein the addition amount of the sodium carbonate is properly increased or decreased along with the change of the acidity of the dicamba technical product, and the pH value of the dicamba sodium salt is controlled to be between 7.0 and 9.0.
(2) Ingredients
The samples were weighed according to the following compounding schedule:
Figure DEST_PATH_IMAGE006
accurately weighing the above materials (except dicamba sodium salt), and mixing well for later use.
The other steps are the same as in example 1.
Example 4: the herbicide contains 42.5% of dicamba and 12.5% of nicosulfuron
The preparation method comprises the following steps:
(1) synthesis of dicamba sodium salt
Putting 120kg of dicamba technical material and 35.2kg of sodium carbonate into a trough type kneader, adding 1.2kg of water after uniformly stirring, continuously kneading, carrying out rotary extrusion granulation after standing for about 60min, bagging after the granulation is finished, and standing for later use;
wherein the addition amount of the sodium carbonate is properly increased or decreased along with the change of the acidity of the dicamba technical product, and the pH value of the dicamba sodium salt is controlled to be between 7.0 and 9.0.
(2) Ingredients
The samples were weighed according to the following compounding schedule:
Figure DEST_PATH_IMAGE008
accurately weighing the above materials (except dicamba sodium salt), and mixing well for later use.
The other steps are the same as in example 1.
The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.

Claims (9)

1. A compound herbicide containing dicamba is characterized in that: the dicamba pesticide comprises a first effective component and a second effective component, wherein the first effective component is 40-60% of dicamba by mass; the second active ingredient is one or a mixture of nicosulfuron and rimsulfuron, the mass percent of the nicosulfuron is 0-15%, and the mass percent of the rimsulfuron is 0-15%.
2. The dicamba-containing compound herbicide as claimed in claim 1, wherein: the adhesive also comprises 1-4% of wetting agent, 1-15% of dispersing agent, 0-10% of acid-base regulator, 0-5% of binder and the balance of filler.
3. The dicamba-containing compound herbicide as claimed in claim 2, wherein: the wetting agent is one or a combination of several of sodium dodecyl sulfate, sodium sulfosuccinate, alkyl succinic acid sulfonate, fatty alcohol-polyoxyethylene ether, sodium alkyl benzene sulfonate and alkyl naphthalene sulfonate.
4. The dicamba-containing compound herbicide as claimed in claim 2, wherein: the dispersing agent is one or a combination of more of alkylphenol polyoxyethylene ether formaldehyde condensate, lignosulfonate, polycarboxylate, naphthalenesulfonate formaldehyde condensate and p-methoxy fatty amido benzene sulfonic acid.
5. The dicamba-containing compound herbicide as claimed in claim 2, wherein: the pH regulator is one or more of ethylenediamine tetraacetic acid, disodium ethylenediamine tetraacetic acid, sodium tripolyphosphate and citric acid.
6. The dicamba-containing compound herbicide as claimed in claim 2, wherein: the binder is one or more of urea, glucose, soft white sugar, polyethylene glycol, soluble starch and sodium carboxymethylcellulose.
7. The dicamba-containing compound herbicide as claimed in claim 2, wherein: the filler is one or a combination of more of sodium sulfate, ammonium sulfate, corn starch, kaolin, light calcium carbonate, talcum powder, wollastonite powder, sodium acetate, potassium chloride, sodium chloride and diatomite.
8. The preparation method of the dicamba-containing compound herbicide as claimed in claim 2, wherein the dicamba-containing compound herbicide comprises the following steps: the process is as follows:
synthesis of dicamba sodium salt: weighing dicamba active compound and sodium carbonate according to a ratio, putting the dicamba active compound and the sodium carbonate into a trough type kneader, adding water after uniformly stirring, continuing kneading, carrying out rotary extrusion granulation after placing for a period of time, and bagging and placing for later use after the granulation is finished;
preparing materials according to a given proportion: weighing the materials according to the following mass percentage, and uniformly mixing for later use; 0-15% of nicosulfuron, 0-15% of rimsulfuron, 1-4% of a wetting agent, 1-15% of a dispersing agent, 0-10% of an acid-base regulator, 0-5% of a binder and the balance of a filler to 100%;
airflow crushing: crushing the mixed materials in a jet mill to ensure that the particle fineness meets the requirement of wet screening, and crushing for later use; the air inlet pressure and the feeding speed are controlled in the air flow crushing process, so that large fluctuation is avoided;
and (3) granulation: adding the powder subjected to jet milling into a kneader, uniformly stirring, adding a dicamba sodium salt wet material with the mass percentage of 40-60%, continuously uniformly stirring, adding water, kneading for about 5min, starting granulation, continuously and uniformly adding the wet material into a rotary extrusion granulator, controlling the feeding speed and the material level in the granulator, and keeping for later use after extrusion;
drying: starting the boiling dryer, preheating to 50 ℃, adding the materials, setting the drying temperature to 65 ℃, and performing screening detection after drying.
9. The preparation method of the dicamba-containing compound herbicide as claimed in claim 8, wherein the dicamba-containing compound herbicide comprises the following steps: the mass ratio of the dicamba technical material to the sodium carbonate is adjusted according to the acid strength of the dicamba technical material, and the pH value of the dicamba sodium salt is controlled to be 7.9-9.0.
CN202010709727.2A 2020-07-22 2020-07-22 Compound herbicide containing dicamba and preparation method thereof Pending CN111758728A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN113519522A (en) * 2021-08-31 2021-10-22 镇江建苏农药化工有限公司 Dicamba-2 methyl-4 chlorodimethylamine salt-based soluble solution and preparation method thereof

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Application publication date: 20201013