CN113854287A - Corn field herbicide composition and preparation method thereof - Google Patents
Corn field herbicide composition and preparation method thereof Download PDFInfo
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- CN113854287A CN113854287A CN202111277791.9A CN202111277791A CN113854287A CN 113854287 A CN113854287 A CN 113854287A CN 202111277791 A CN202111277791 A CN 202111277791A CN 113854287 A CN113854287 A CN 113854287A
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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
- 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
- A01N25/08—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 solids as carriers or diluents
- A01N25/10—Macromolecular compounds
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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
- 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
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- 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
- A01N41/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom
- A01N41/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom containing a sulfur-to-oxygen double bond
- A01N41/10—Sulfones; Sulfoxides
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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
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/66—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms
- A01N43/68—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms with two or three nitrogen atoms directly attached to ring carbon atoms
- A01N43/70—Diamino—1,3,5—triazines with only one oxygen, sulfur or halogen atom or only one cyano, thiocyano (—SCN), cyanato (—OCN) or azido (—N3) group directly attached to a ring carbon atom
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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<
- A01N47/36—Ureas 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
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F251/00—Macromolecular compounds obtained by polymerising monomers on to polysaccharides or derivatives thereof
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Abstract
The application relates to the field of herbicides, and particularly discloses a corn field herbicide composition and a preparation method thereof. The corn field herbicide composition is prepared from the following raw materials in parts by weight: 4-6 parts of nicosulfuron, 8-12 parts of mesotrione, 18-22 parts of atrazine, 0.2-0.5 part of safener, 15-20 parts of emulsifier, 2-2 parts of OP-151, 0.5-1 part of wetting agent, 40-50 parts of soybean oil, 2-3 parts of carboxymethyl starch, 3-5 parts of sodium lignosulfonate, 1-2 parts of hydroxypropyl methyl cellulose, 0.3-0.6 part of water-soluble cross-linking agent, 1-2 parts of water-retaining agent, and the average particle size of nicosulfuron, mesotrione and atrazine is 2-3 mu m. The corn field herbicide composition has high control efficiency on common weeds in the corn field, has high stability and meets market requirements.
Description
Technical Field
The application relates to the field of herbicides, in particular to a corn field herbicide composition and a preparation method thereof.
Background
Corn is an annual herbaceous plant of the family poaceae. Compared with wheat and rice, the corn has strong drought tolerance, cold tolerance and barrenness tolerance and higher nutritional value, so that the corn becomes one of the most excellent and important grain crops in the world. In addition, corn is also an important feed source in animal husbandry, aquaculture and the like. The corn has rich resources, low price and easy acquisition, so that the corn has wide application prospect. However, during the corn planting and growing process, corn seedlings are easily damaged by weeds, so that the yield of corn is remarkably reduced, and therefore, the development and application of herbicides applied to corn fields are a hot topic for a long time.
Nicosulfuron is a systemic herbicide, can be absorbed by stems, leaves and roots of weeds, and then is conducted in plants, so that sensitive plants are caused to stop growing, the stems and leaves are faded and gradually withered, and the sensitive plants die in 20-25 days generally. Nicosulfuron is one of the most widely used herbicides at present.
In order to increase the weed control spectrum of the herbicide and reduce the generation of weed drug resistance, nicosulfuron is often compounded with mesotrione and atrazine for use. The formula is the herbicide which is widest in application range at present, can be applied to mesotrione, nicosulfuron and atrazine in the 3-5 leaf stage and the 2-4 leaf stage of the weeds of the corns, can effectively prevent and kill off annual broadleaf weeds and gramineous weeds in the corn fields, has good safety to the corns, can weed cleanly and thoroughly, and is not easy to rebound.
The oil suspending agent is a pesticide formulation with high competitiveness, and the nicosulfuron, the mesotrione and the atrazine are commonly prepared into the oil suspending agent for use. However, the herbicide may have the problems of agglomeration and caking during production, storage and use, so that the control effect is poor after the herbicide is applied to a corn field by farmers. In addition, the herbicide has short retention time on the ground surface after being sprayed on the corn field, and is easy to permeate into the ground surface, so that the effect of the herbicide on preventing weeds is obviously reduced. Therefore, the development of a stable herbicide for corn fields with excellent weed control effect is urgently needed.
Disclosure of Invention
In order to improve the stability of the corn field herbicide and improve the weed control efficiency of the corn field herbicide, the application provides a corn field herbicide composition and a preparation method thereof.
In a first aspect, the present application provides a corn field herbicide composition, which adopts the following technical scheme:
the corn field herbicide composition is prepared from the following raw materials in parts by weight: 4-6 parts of nicosulfuron, 8-12 parts of mesotrione, 18-22 parts of atrazine, 0.2-0.5 part of safener, 15-20 parts of emulsifier, 2-2 parts of OP-151, 0.5-1 part of wetting agent, 40-50 parts of soybean oil, 2-3 parts of carboxymethyl starch, 3-5 parts of sodium lignosulfonate, 1-2 parts of hydroxypropyl methyl cellulose, 0.3-0.6 part of water-soluble cross-linking agent, 1-2 parts of water-retaining agent, and the average particle size of nicosulfuron, mesotrione and atrazine is 2-3 mu m.
By adopting the technical scheme, the corn field herbicide composition has a wider weed control spectrum, and can be used for treating common gramineous weeds in corn fields: large crabgrass, barnyard grass, green bristlegrass, and broadleaf weeds: amaranthus retroflexus has high prevention efficiency. The control efficiency range of the pesticide to the large crabgrass is 95.01-99.9%; the control efficiency range of the barnyard grass is 94.25 to 98.23 percent; the control efficiency range of the green bristlegrass herb is 96.22 to 99.9 percent; the control efficiency range of the amaranthus retroflexus is 85.38-89.30%. In addition, the plant height inhibition rate of the herbicide composition for corn fields is low and is negative, which indicates that the herbicide composition for corn fields has a certain promotion effect on the growth of corn, and the plant height inhibition rate of the herbicide composition for corn fields ranges from-6.5 to 0.3 percent. In addition, it has high suspension rate in the range of 84.1-96.1%. In the application, the synergistic effect of the raw materials improves the weed control efficiency of the corn field herbicide composition, improves the stability of the corn field herbicide composition, and meets the market demand.
In the application, the nicosulfuron, the mesotrione and the atrazine are compounded, so that the weed control spectrum of the corn field herbicide composition is increased; the safety of the corn field herbicide on corn is improved by adding the safener; and the synergistic effect of the carboxymethyl starch, the sodium lignosulfonate, the hydroxypropyl methyl cellulose and the cross-linking agent obviously improves the weed control efficiency of the corn field herbicide composition.
The applicant finds that carboxymethyl starch, sodium lignosulfonate and hydroxypropyl methyl cellulose are all high molecular polymers and play a role in thickening the corn field herbicide composition, in addition, the carboxymethyl starch and the hydroxypropyl methyl cellulose are easy to form films, and under the action of a cross-linking agent, the three high molecular substances form a macromolecular substance with a three-dimensional net structure through intermolecular force, so that the corn field herbicide composition is facilitated to form a medicinal film on the surface of a corn field, the weed prevention efficiency of the corn field herbicide composition is improved, and meanwhile, the suspension rate of the corn field herbicide composition can be further improved, and the stability of the corn field herbicide composition is improved.
Optionally, the safener is one or more of isoxadifen and cyclopropanesulfonamide.
By adopting the technical scheme, the safener is simple and easy to obtain, and the plant height inhibition rate of the corn field herbicide composition on corn can be effectively reduced.
Optionally, the safener is cyclopropanesulfonamide.
By adopting the technical scheme, compared with the isoxadifen, the cypionesulfonamide is used as a safener, so that the plant height inhibition rate of the corn field herbicide composition on corn can be further reduced.
Optionally, the emulsifier is one or more of calcium dodecylbenzene sulfonate and castor oil polyoxyethylene ether.
By adopting the technical scheme, the emulsifier raw materials are simple and easy to obtain, and the corn field herbicide composition has higher suspension rate, so that the stability of the corn field herbicide composition is improved.
Optionally, the emulsifier is a mixture of calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether, and the mass ratio of the calcium dodecyl benzene sulfonate to the castor oil polyoxyethylene ether is 4: 1.
By adopting the technical scheme, compared with the method of singly taking calcium dodecyl benzene sulfonate or castor oil polyoxyethylene ether as an emulsifier, the suspension rate of the corn field herbicide composition can be further improved.
Optionally, the cross-linking agent is acrylic acid grafted chitosan oligosaccharide.
By adopting the technical scheme, the weed control efficiency of the corn field herbicide composition can be remarkably improved, and the acrylic acid grafted chitosan oligosaccharide is a water-soluble degradable cross-linking agent, is applied to the corn field herbicide composition, and is not easy to pollute the environment.
Optionally, the acrylic acid grafted chitosan oligosaccharide is prepared from the following raw materials in parts by weight: 10-12 parts of chitosan oligosaccharide, 10-6 parts of EDC5, 2-4 parts of NHS, 30-35 parts of water, 8-10 parts of acrylic acid and 120 parts of ethanol.
By adopting the technical scheme, the raw materials of the acrylic acid grafted chitosan oligosaccharide are simple and easy to obtain.
Optionally, the acrylic acid grafted chitosan oligosaccharide is prepared by the following method:
step S1: dissolving chitosan oligosaccharide in water, adjusting pH to 4-5, adding EDC and NHS, stirring to mix uniformly, adding acrylic acid, and reacting for 70-80h under stirring to obtain a crude product;
and step S2, adding the crude product into ethanol, stirring for 10-15min, filtering, and drying to obtain the acrylic acid grafted chitosan oligosaccharide.
By adopting the technical scheme, the preparation method of the acrylic acid grafted chitosan oligosaccharide is simple and easy to operate, and the prepared acrylic acid grafted chitosan oligosaccharide is stable.
Optionally, the water-retaining agent is one or more of glycerol, propylene glycol and sorbitol.
By adopting the technical scheme, the weed control efficiency of the corn field herbicide composition can be improved, and the performance detection result of the corn field herbicide composition is not influenced by the glycerol, the propylene glycol and the sorbitol.
In a second aspect, the application provides a preparation method of a corn field herbicide composition, which adopts the following technical scheme: a preparation method of a corn field herbicide composition comprises the following steps:
step Sa: dissolving an emulsifier in soybean oil, adding nicosulfuron, mesotrione and atrazine under stirring, sequentially adding a safener, OP-15 and a wetting agent, and stirring for 10-15min to obtain a mixture I;
and Sb: uniformly mixing carboxymethyl starch, sodium lignosulfonate, hydroxypropyl methylcellulose, a cross-linking agent and a water-retaining agent, adding into the mixture I, stirring for 40-50min, shearing for 20-30min, and grinding until the average particle size of nicosulfuron, mesotrione and atrazine is 2-3 μm to obtain the corn field herbicide composition.
By adopting the technical scheme, the preparation steps of the corn field herbicide composition are simple, the operation is easy, and the stability of the corn field herbicide composition is improved.
In summary, the present application has at least the following beneficial effects:
1. according to the corn field herbicide composition, a high molecular compound with a three-dimensional net structure is formed through the synergistic effect of carboxymethyl starch, sodium lignosulfonate, hydroxypropyl methyl cellulose and a water-soluble cross-linking agent, so that a pesticide film is easily formed on the surface of a corn field by the corn field herbicide composition, the weed control efficiency of the corn field herbicide composition is improved, and meanwhile, OP-15 is added, so that the suspension rate of the corn field herbicide composition is remarkably improved, and the stability of the corn field herbicide composition is improved;
2. the acrylic acid grafted chitosan oligosaccharide is used as the cross-linking agent, so that the weed control efficiency of the corn field herbicide composition is further improved, and meanwhile, the acrylic acid grafted chitosan oligosaccharide is a water-soluble degradable cross-linking agent, is applied to the corn field herbicide composition, and is not easy to pollute the environment.
Detailed Description
The present invention will be described in further detail with reference to examples.
Raw materials
The chitosan oligosaccharide is selected from Shandong Nuanli Biotech limited; castor oil polyoxyethylene ether is dn2301 type, and Shandong Dennuo New Material science and technology company; the calcium dodecylbenzene sulfonate is selected from Shandong Cuihua Biotech limited; OP-15 and is selected from Kapler Biotech, Inc., Shandong; the soybean oil is 283 and is selected from Xian Jinxiang pharmaceutic adjuvant limited company; the carboxymethyl starch is selected from chemical industry Co., Ltd; the sodium lignosulfonate is selected from chemical Limited of Jinnan Hongwang; the hydroxypropyl methylcellulose is selected from Jinniu chemical Co., Ltd in Jinan; the polyether modified silicone oil (YNE408) is selected from Jenno chemical Co., Ltd.
Preparation example
TABLE 1 raw material content (kg) of acrylic acid-grafted Chitosan oligosaccharide in preparation examples 1 to 4
| Raw materials | Preparation example 1 | Preparation example 2 | Preparation example 3 | Preparation example 4 |
| Chitosan oligosaccharide | 10 | 11 | 11.5 | 12 |
| EDC | 6 | 5.2 | 5.4 | 5 |
| NHS | 2.6 | 3 | 2 | 4 |
| Water (W) | 32 | 34 | 35 | 30 |
| Acrylic acid | 10 | 9 | 8 | 9.5 |
| Ethanol | 110 | 115 | 120 | 100 |
Note: EDC is 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride; NHS for N-hydroxy succinimide.
Preparation example 1
The raw material content of the acrylic acid grafted chitosan oligosaccharide is shown in table 1.
An acrylic acid grafted chitosan oligosaccharide, which is prepared by the following method:
step S1: adding water into a reaction kettle, dissolving chitosan oligosaccharide in the water, adjusting the pH value of a chitosan oligosaccharide solution to 4 by using 20% hydrochloric acid, adding EDC and NHS, stirring until the mixture is uniformly mixed, adding acrylic acid, and reacting for 80 hours under the stirring condition to obtain a crude product; and step S2, adding the crude product into ethanol, stirring for 10min, filtering, and drying to obtain the acrylic acid grafted chitosan oligosaccharide.
Preparation example 2
An acrylic acid-grafted chitosan oligosaccharide which is different from that of preparation example 1 in the content of raw materials, as shown in table 1;
it is also distinguished from preparation example 1 by the fact that it is prepared under different preparation conditions by the following method:
step S1: adding water into a reaction kettle, dissolving chitosan oligosaccharide in the water, adjusting the pH value of a chitosan oligosaccharide solution to 4.5 by using 20% hydrochloric acid, adding EDC and NHS, stirring until the mixture is uniformly mixed, adding acrylic acid, and reacting for 75 hours under the stirring condition to obtain a crude product; and step S2, adding the crude product into ethanol, stirring for 15min, filtering, and drying to obtain the acrylic acid grafted chitosan oligosaccharide.
Preparation example 3
An acrylic acid-grafted chitosan oligosaccharide which is different from that of preparation example 2 in the content of raw materials, as shown in table 1;
it is also distinguished from preparation example 2 in that, unlike the preparation process, it is prepared by the following process:
step S1: adding water into a reaction kettle, dissolving chitosan oligosaccharide in the water, adjusting the pH value of a chitosan oligosaccharide solution to 5 by using 20% hydrochloric acid, adding EDC and NHS, stirring until the mixture is uniformly mixed, adding acrylic acid, and reacting for 70 hours under the stirring condition to obtain a crude product; and step S2, adding the crude product into ethanol, stirring for 12min, filtering, and drying to obtain the acrylic acid grafted chitosan oligosaccharide.
Preparation example 4
An acrylic acid-grafted chitosan oligosaccharide which is different from that of preparation example 2 in the content of raw materials, as shown in table 1;
it is also distinguished from preparation example 2 by the fact that it is prepared under different preparation conditions by the following method:
step S1: adding water into a reaction kettle, dissolving chitosan oligosaccharide in the water, adjusting the pH value of a chitosan oligosaccharide solution to 4.8 by using 20% hydrochloric acid, adding EDC and NHS, stirring until the mixture is uniformly mixed, adding acrylic acid, and reacting for 72 hours under the stirring condition to obtain a crude product; and step S2, adding the crude product into ethanol, stirring for 14min, filtering, and drying to obtain the acrylic acid grafted chitosan oligosaccharide.
Examples
TABLE 2 raw material content (kg) of the corn field herbicide composition of examples 1-4
Example 1
A corn field herbicide composition comprises the raw materials shown in the table 2.
And the safener is cyclopropanesulfonamide;
the emulsifier is calcium dodecyl benzene sulfonate;
the wetting agent is polyether modified silicone oil (YNE 408);
the water-retaining agent is glycerol;
the cross-linking agent is acrylic acid grafted chitosan oligosaccharide which is prepared from the preparation example 1.
A preparation method of a corn field herbicide composition comprises the following steps:
step Sa: adding soybean oil into a stirrer, dissolving an emulsifier in the soybean oil, adding nicosulfuron, mesotrione and atrazine under the stirring condition, sequentially adding a safener, OP-15 and a wetting agent, and stirring for 10min to obtain a mixture I;
and Sb: stirring carboxymethyl starch, sodium lignosulfonate, hydroxypropyl methyl cellulose, a cross-linking agent and a water-retaining agent in a stirrer until the materials are uniformly mixed to obtain a mixture II, then adding the mixture II into the mixture I, stirring for 45min to obtain a primary product, adding the primary product into a shearing kettle, shearing for 25min, and carrying out three-stage grinding until the average particle size of nicosulfuron, mesotrione and atrazine is 2.5 mu m to obtain the corn field herbicide composition.
Example 2
A corn field herbicide composition which is different from that in example 1 in the content of raw materials, wherein the content of the raw materials is shown in table 2;
it is also different from example 1 in the preparation method.
A preparation method of a corn field herbicide composition comprises the following steps:
step Sa: adding soybean oil into a stirrer, dissolving an emulsifier in the soybean oil, adding nicosulfuron, mesotrione and atrazine under the stirring condition, sequentially adding a safener, OP-15 and a wetting agent, and stirring for 15min to obtain a mixture I;
and Sb: stirring carboxymethyl starch, sodium lignosulfonate, hydroxypropyl methyl cellulose, a cross-linking agent and a water-retaining agent in a stirrer until the materials are uniformly mixed to obtain a mixture II, then adding the mixture II into the mixture I, stirring for 40min to obtain a primary product, adding the primary product into a shearing kettle, shearing for 20min, and carrying out three-stage grinding until the average particle size of nicosulfuron, mesotrione and atrazine is 3 mu m to obtain the corn field herbicide composition.
Example 3
A corn field herbicide composition which is different from that in example 1 in the content of raw materials, wherein the content of the raw materials is shown in table 2;
it is also different from example 1 in the preparation method.
A preparation method of a corn field herbicide composition comprises the following steps:
step Sa: adding soybean oil into a stirrer, dissolving an emulsifier in the soybean oil, adding nicosulfuron, mesotrione and atrazine under the stirring condition, sequentially adding a safener, OP-15 and a wetting agent, and stirring for 12min to obtain a mixture I;
and Sb: stirring carboxymethyl starch, sodium lignosulfonate, hydroxypropyl methyl cellulose, a cross-linking agent and a water-retaining agent in a stirrer until the materials are uniformly mixed to obtain a mixture II, then adding the mixture II into the mixture I, stirring for 50min to obtain a primary product, adding the primary product into a shearing kettle, shearing for 30min, and carrying out three-stage grinding until the average particle size of nicosulfuron, mesotrione and atrazine is 2 microns to obtain the corn field herbicide composition.
Example 4
A corn field herbicide composition which differs from that of example 3 in the content of raw materials, which is shown in table 2;
it is also different from example 3 in the method of preparation.
A preparation method of a corn field herbicide composition comprises the following steps:
step Sa: adding soybean oil into a stirrer, dissolving an emulsifier in the soybean oil, adding nicosulfuron, mesotrione and atrazine under the stirring condition, sequentially adding a safener, OP-15 and a wetting agent, and stirring for 14min to obtain a mixture I;
and Sb: stirring carboxymethyl starch, sodium lignosulfonate, hydroxypropyl methyl cellulose, a cross-linking agent and a water-retaining agent in a stirrer until the materials are uniformly mixed to obtain a mixture II, then adding the mixture II into the mixture I, stirring for 48min to obtain a primary product, adding the primary product into a shearing kettle, shearing for 28min, and carrying out three-stage grinding until the average particle size of nicosulfuron, mesotrione and atrazine is 2 microns to obtain the corn field herbicide composition.
Example 5
A corn field herbicide composition which differs from example 3 in that the cyclopropanesulfonamide is replaced by an equal amount of isoxadifen, the remainder being the same as in example 3.
Example 6
A corn field herbicide composition which differs from example 3 in that the calcium dodecylbenzenesulfonate is replaced with an equal amount of castor oil polyoxyethylene ether, and the remainder is the same as in example 3.
Example 7
A corn field herbicide composition is different from that in the embodiment 3 in that calcium dodecyl benzene sulfonate is replaced by a mixture of equivalent calcium dodecyl benzene sulfonate and castor oil polyoxyethylene ether in a mass ratio of 4:1, and the rest is the same as that in the embodiment 3.
Example 8
A corn field herbicide composition which is different from that of example 7 in that acrylic acid-grafted chitosan oligosaccharide is prepared from preparation example 2, and the rest is the same as that of example 7.
Example 9
A corn field herbicide composition which is different from that of example 8 in that acrylic acid-grafted chitosan oligosaccharide is prepared in preparation example 3, and the rest is the same as that of example 8.
Example 10
A corn field herbicide composition which is rated differently from example 8 in that an acrylic acid-grafted chitosan oligosaccharide was prepared as in preparation example 4, and the rest is the same as example 8.
Comparative example
Comparative example 1
A corn field herbicide composition, which is different from the herbicide composition in the embodiment 8 in that OP-15 is not added in the raw materials of the corn field herbicide composition, and the rest is the same as the herbicide composition in the embodiment 8.
Comparative example 2
A corn field herbicide composition, which is different from the corn field herbicide composition in the embodiment 8 in that carboxymethyl starch is not added in the raw materials of the corn field herbicide composition, and the rest is the same as the corn field herbicide composition in the embodiment 8.
Comparative example 3
A corn field herbicide composition, which is different from the herbicide composition in the embodiment 8 in that sodium lignosulfonate is not added into the raw materials of the corn field herbicide composition, and the rest is the same as the herbicide composition in the embodiment 8.
Comparative example 4
A corn field herbicide composition, which is different from the herbicide composition in the embodiment 8 in that hydroxypropyl methylcellulose is not added in the raw materials of the corn field herbicide composition, and the rest is the same as the herbicide composition in the embodiment 8.
Comparative example 5
A corn field herbicide composition, which is different from the embodiment 8 in that the raw materials of the corn field herbicide composition are not added with acrylic acid grafted chitosan oligosaccharide, and the rest is the same as the embodiment 8.
Comparative example 6
A corn field herbicide composition, which is different from the embodiment 8 in that carboxymethyl starch, sodium lignosulphonate, hydroxypropyl methyl cellulose and acrylic acid grafted chitosan oligosaccharide are not added into the raw materials of the corn field herbicide composition, and the rest is the same as the embodiment 8.
Comparative example 7
A corn field herbicide composition, which is different from that of example 8 in that, in step Sb, nicosulfuron, mesotrione, and atrazine were ground to have an average particle size of 5 μm, and the rest was the same as in example 8.
Performance test
100ml of the corn field herbicide compositions prepared in examples 1-10 and comparative examples 1-7 are taken respectively, and 35 kg of water is added to prepare 17 herbicide diluents for later use.
Spraying the stems and leaves of the 17 kinds of diluents to the corns and the weeds in a 3-5 leaf stage and a 2-4 leaf stage of the corns and the weeds respectively. And a control group is set, and the same amount of clear water is sprayed. Wherein the corn variety is Tayu No. 14; the weeds are respectively common gramineous weeds of crab grass, barnyard grass, green bristlegrass herb and broad-leaved weeds of amaranthus retroflexus in the corn field. Investigating the plant height of corn and the fresh weight of weeds at 15 days after application of the herbicide respectively, and calculating the plant height inhibition rate of the herbicide diluent on the corn and the weed control efficiency according to the following formulas respectively, wherein the plant height inhibition rate of the corn is calculated according to the formula 1; the fresh weight control efficiency of the weeds is calculated according to the formula 2. The test investigation method is carried out according to the national standard 'pesticide field efficacy test criterion (I) herbicide control corn field weed'. The results are shown in Table 3.
The dosage of the 17 herbicide diluents is 48g.a.i/h square meter.
The plant height inhibition rate of corn is (Ha-Hb)/Ha 100 percent formula 1
Wherein Ha is the corn plant height 15 days after the blank control group; hb is the plant height of the corn 15 days after application.
Efficiency of protection (1-PT/CK) × 100% equation 2
Wherein PT is the survival number (fresh weight) of the weeds after the herbicide diluent is treated; CK is the survival number (fresh weight) of the weeds in the control group.
The suspension rates of the corn field herbicide compositions prepared in examples 1-10 and comparative examples 1-7 were measured according to GB/T14825-2006 "method for measuring suspension rates of pesticides", and the measurement results are shown in Table 3.
TABLE 3 test results
As can be seen from table 3, the corn field herbicide composition of the present application is effective against common grassy weeds in corn fields: large crabgrass, barnyard grass, green bristlegrass, and broadleaf weeds: amaranthus retroflexus has high fresh weight prevention efficiency. Wherein the control efficiency range of the crabgrass is 95.01-99.9%; the control efficiency range of the barnyard grass is 94.25 to 98.23 percent; the control efficiency range of the green bristlegrass herb is 96.22 to 99.9 percent; the control efficiency range of the amaranthus retroflexus is 85.38-89.30%. The corn field herbicide composition has a certain promotion effect on the growth of corn, and the inhibition rate of the herbicide composition on the height of corn plants ranges from-6.5% to 0.3%. In addition, the corn field herbicide composition has high suspension rate, and the suspension rate ranges from 84.1% to 96.1%. The herbicide composition for the corn field can prevent and control common weeds in the corn field, has a wide weed control spectrum, has a certain promotion effect on the growth of corn, and has a high suspension rate. In the application, the synergistic effect of the raw materials remarkably improves the weed control efficiency and the weed control stability of the corn field herbicide composition, and meets the market demand.
Comparing comparative example 1 with example 8, it can be seen that the suspension rate of the corn field herbicide composition prepared in example 8 is 96.1%; the corn field herbicide composition prepared in comparative example 1 had a suspension rate of 72.3%. Compared with example 8, no OP-15 is added in comparative example 1, which shows that the addition of OP-15 can obviously improve the suspension rate of the corn field herbicide composition. OP-15 is an auxiliary dispersant, OP-15 can effectively reduce mutual agglomeration among particles, so that the stability of a dispersion system is maintained, the flocculation degree of the corn field herbicide is reduced, the steric hindrance and electrostatic repulsion among particles are increased, the spatial network structure is weakened, the thixotropy is reduced, the recovery time after damage is short, the layering and caking phenomena of the corn field herbicide composition are effectively reduced, and the stability of the corn field herbicide composition is improved. In addition, the addition of OP-15 further improves the control efficiency of the corn field herbicide composition on weeds.
Comparing comparative examples 2 to 6 with example 8, the corn field herbicide composition prepared in example 8 has control efficiency of 99.9%, 98.82%, 99.9% and 89.3% for crab grass, barnyard grass, green bristlegrass and redroot amaranth respectively; the control efficiencies of the corn field herbicide composition prepared in comparative example 2 on crab grass, barnyard grass, green bristlegrass and redroot amaranth were 85.63%, 88.79%, 93.74% and 78.43%, respectively; the control efficiencies of the corn field herbicide composition prepared in comparative example 3 on crab grass, barnyard grass, green bristlegrass and redroot amaranth were 87.54%, 90.41%, 95.04% and 79.68%, respectively; the control efficiencies of the corn field herbicide composition prepared in comparative example 4 to crab grass, barnyard grass, green bristlegrass and redroot amaranth were 85.92%, 88.64%, 93.38% and 78.07%, respectively; the control efficiencies of the corn field herbicide composition prepared in comparative example 5 to crab grass, barnyard grass, green bristlegrass and redroot amaranth were 81.96%, 87.32%, 92.79% and 76.11%, respectively; the corn field herbicide compositions prepared in comparative example 6 had control efficiencies of 76.25%, 85.69%, 90.78%, and 73.08% for crab grass, barnyard grass, green bristlegrass, and amaranthus retroflexus, respectively. It can be seen that the herbicidal compositions for corn fields in comparative examples 2 to 6 all had significantly reduced control efficiency against weeds compared to the herbicidal compositions for corn fields prepared in example 8.
Carboxymethyl starch and hydroxypropyl methyl cellulose are all high molecular compounds which are easy to form films, and after the carboxymethyl starch and the hydroxypropyl methyl cellulose are added into the corn field herbicide composition, the corn field herbicide composition is applied to fields, and a medicinal film is easy to form on the ground surface, so that the weed control efficiency of the corn field herbicide composition can be obviously improved. Under the action of cross-linking agent acrylic acid grafted chitosan oligosaccharide, carboxymethyl starch, hydroxypropyl methylcellulose and sodium lignin sulfonate can form a liquid film with a three-dimensional network structure due to intermolecular force, so that the weed control efficiency of the corn field herbicide composition is further improved. In addition, the sodium lignosulfonate can improve the dispersibility of the corn field herbicide composition, so that the suspension rate of the corn field herbicide composition is further increased, and the stability of the corn field herbicide composition is further improved.
As can be seen from comparative example 7 and example 8, the corn field herbicide composition prepared in comparative example 7 had a suspension rate of 61.2%; the corn field herbicide composition prepared in example 8 had a suspension rate of 96.1%. The fact shows that when the average particle size of the nicosulfuron, the mesotrione and the atrazine in the herbicide composition for the corn field is 2-3 mu m, the suspension rate is remarkably reduced, and the control efficiency of the herbicide composition for the corn field is reduced. The smaller the average particle size of nicosulfuron, mesotrione and atrazine in the corn field herbicide composition is, the higher the stability of the herbicide composition is, so that the prevention efficiency of the herbicide composition on weeds is improved, and the market demand is met.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (10)
1. The corn field herbicide composition is characterized by being prepared from the following raw materials in parts by weight: 4-6 parts of nicosulfuron, 8-12 parts of mesotrione, 18-22 parts of atrazine, 0.2-0.5 part of safener, 15-20 parts of emulsifier, 2-2 parts of OP-151, 0.5-1 part of wetting agent, 40-50 parts of soybean oil, 2-3 parts of carboxymethyl starch, 3-5 parts of sodium lignosulfonate, 1-2 parts of hydroxypropyl methyl cellulose, 0.3-0.6 part of water-soluble cross-linking agent, 1-2 parts of water-retaining agent, and the average particle size of nicosulfuron, mesotrione and atrazine is 2-3 mu m.
2. The corn field herbicide composition as claimed in claim 1, wherein the safener is one or more of isoxadifen and cyprosulfamide.
3. The corn field herbicide composition as claimed in claim 2, wherein the safener is cyprosulfamide.
4. The corn field herbicide composition as claimed in claim 1, wherein the emulsifier is one or more of calcium dodecylbenzene sulfonate and castor oil polyoxyethylene ether.
5. The corn field herbicide composition as claimed in claim 4, wherein the emulsifier is a mixture of calcium dodecylbenzene sulfonate and castor oil polyoxyethylene ether, and the mass ratio of the calcium dodecylbenzene sulfonate to the castor oil polyoxyethylene ether is 4: 1.
6. The corn field herbicide composition as claimed in claim 1, wherein the cross-linking agent is acrylic acid grafted chitosan oligosaccharide.
7. The corn field herbicide composition as claimed in claim 6, wherein the acrylic acid grafted chitosan oligosaccharide is prepared from the following raw materials in parts by weight: 10-12 parts of chitosan oligosaccharide, 5-6 parts of EDC, 2-4 parts of NHS, 30-35 parts of water, 8-10 parts of acrylic acid and 120 parts of ethanol.
8. The corn field herbicide composition as claimed in claim 7, wherein the acrylic acid grafted chitosan oligosaccharide is prepared by the following method:
step S1: dissolving chitosan oligosaccharide in water, adjusting pH to 4-5, adding EDC and NHS, stirring to mix uniformly, adding acrylic acid, and reacting for 70-80h under stirring to obtain a crude product;
and step S2, adding the crude product into ethanol, stirring for 10-15min, filtering, and drying to obtain the acrylic acid grafted chitosan oligosaccharide.
9. The corn field herbicide composition as claimed in claim 1, wherein the water retention agent is one or more of glycerin, propylene glycol and sorbitol.
10. A method of preparing a corn field herbicide composition as claimed in any one of claims 1 to 9, comprising the steps of:
step Sa: dissolving an emulsifier in soybean oil, adding nicosulfuron, mesotrione and atrazine under stirring, sequentially adding a safener, OP-15 and a wetting agent, and stirring for 10-15min to obtain a mixture I;
and Sb: uniformly mixing carboxymethyl starch, sodium lignosulfonate, hydroxypropyl methylcellulose, a cross-linking agent and a water-retaining agent, adding into the mixture I, stirring for 40-50min, shearing for 20-30min, and grinding until the average particle size of nicosulfuron, mesotrione and atrazine is 2-3 μm to obtain the corn field herbicide composition.
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