CN112806361B - Carbon adsorption 4-hydroxycoumarin herbicide safety additive and application thereof in treatment of herbicide side effects - Google Patents
Carbon adsorption 4-hydroxycoumarin herbicide safety additive and application thereof in treatment of herbicide side effects Download PDFInfo
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- CN112806361B CN112806361B CN201911129990.8A CN201911129990A CN112806361B CN 112806361 B CN112806361 B CN 112806361B CN 201911129990 A CN201911129990 A CN 201911129990A CN 112806361 B CN112806361 B CN 112806361B
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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
- A01N25/32—Ingredients for reducing the noxious effect of the active substances to organisms other than pests, e.g. toxicity reducing compositions, self-destructing compositions
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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
- A01N37/00—Biocides, 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
- A01N37/18—Biocides, 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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
- A01N37/26—Biocides, 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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof containing the group; Thio analogues thereof
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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
- A01N37/00—Biocides, 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
- A01N37/44—Biocides, 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 nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
- A01N37/48—Nitro-carboxylic acids; Derivatives thereof
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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
- A01N39/00—Biocides, pest repellants or attractants, or plant growth regulators containing aryloxy- or arylthio-aliphatic or cycloaliphatic compounds, containing the group or, e.g. phenoxyethylamine, phenylthio-acetonitrile, phenoxyacetone
- A01N39/02—Aryloxy-carboxylic acids; Derivatives thereof
- A01N39/04—Aryloxy-acetic acids; Derivatives thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- 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
- A01N41/04—Sulfonic acids; Derivatives thereof
- A01N41/06—Sulfonic acid amides
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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
- 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
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/60—1,4-Diazines; Hydrogenated 1,4-diazines
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/22—Improving land use; Improving water use or availability; Controlling erosion
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
- Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures
Abstract
The invention relates to a carbon adsorption 4-hydroxycoumarin herbicide safety additive and application thereof in treatment of side effects of herbicides, belonging to the technical field of herbicides. The carbon-adsorption 4-hydroxycoumarin herbicide safety additive comprises carbon-adsorption 4-hydroxycoumarin and carbon-adsorption polyglutamic acid, and the two are matched for use, so that the additive can repair three types of chemical injury of explicit type, implicit type and residual type caused by using the herbicide, and solve the problems of overproof chemical residue in soil, dead seedling, rotten root, low atrophy, stiff seedling, yellow leaf, dry tip, imbalance in photosynthesis, dehydration, fertilizer removal and other variation symptoms in the seedling stage of crops. After the carbon adsorption 4-hydroxycoumarin herbicide safety additive is sprayed for 40 hours, crops basically recover normal growth, and residues of the herbicide on the crops and soil can be eliminated or decomposed.
Description
Technical Field
The invention relates to a carbon adsorption 4-hydroxycoumarin herbicide safety additive and application thereof in treatment of side effects of herbicides, belonging to the technical field of herbicides.
Background
Farmland weeds are a large category of important biological disasters seriously damaging agricultural production, and farmland chemical weeding is an important measure which is most depended on by farmers at present. The herbicide is easy to cause phytotoxicity when being used, and the phytotoxicity of the herbicide can be classified into three types of acute dominant phytotoxicity, recessive phytotoxicity and residual phytotoxicity. (1) Dominance has the characteristics of quick occurrence of phytotoxicity and obvious symptoms, and the phytotoxicity symptoms appear a few hours or 1 day after the application of the medicine. The damaged leaves have spots, scorching, perforation, deformity, withering, yellowing, green loss and dead seedling and root rot in the seedling stage of crops. (2) Recessive phytotoxicity, atrophy and lack of growth, stiff seedlings, yellow leaves, dry tips, photosynthesis disorder and the like. The growth and development of crops are obviously hindered, and the yield and the quality are reduced. (3) Residual phytotoxicity is not obvious in season crop phytotoxicity of pesticide application, and pesticides remaining in soil have phytotoxicity and stubble changing difficulty on sensitive crops of next crop. In the large-area use of the herbicide, the causes of phytotoxicity of crops are various, some of the phytotoxicity can be avoided, some of the phytotoxicity can be difficult to avoid, and the residual amount and phytotoxicity of the herbicide are very severe.
The Chinese patent application with the publication number of CN 1965652A discloses a herbicide safety additive, which is prepared from 0.01-5 wt% of 4-hydroxycoumarin and 95-99.99 wt% of turpentine. However, the effect of the safety additive on herbicide removal is limited, and no safety additive with good effect on wheat herbicide removal exists at present.
Disclosure of Invention
The invention also provides a carbon adsorption 4-hydroxycoumarin herbicide safety additive, which can eliminate or decompose the residue of the herbicide on crops; especially can prevent the herbicide hazard of wheat and can remove the residual hazard of the herbicide of wheat.
The invention aims to provide an application of a carbon adsorption 4-hydroxycoumarin herbicide safety additive in treatment of side effects of herbicides, which can prevent the side effects of herbicides such as tribenuron-methyl, acetochlor, nicosulfuron, atrazine, 2.4 d isooctyl ester, fomesafen, mesotrione, quizalofop-p-ethyl, marshall butachlor, bensulfuron-methyl, pyrazosulfuron-ethyl, fluoroglycofen-ethyl and the like, and promote the growth of crops such as wheat, corn, soybean, rice and the like.
In order to achieve the purpose, the invention adopts the technical scheme that:
a carbon-adsorbed 4-hydroxycoumarin herbicide safety additive comprises, by weight, 0.001-5% of carbon-adsorbed 4-hydroxycoumarin and 95-99.999% of carbon-adsorbed polyglutamic acid.
The carbon-adsorption 4-hydroxycoumarin herbicide safety additive comprises carbon-adsorption 4-hydroxycoumarin and carbon-adsorption polyglutamic acid, and the two are matched for use, so that the additive can repair three types of chemical injury of explicit type, implicit type and residual type caused by using the herbicide, and solve the problems of overproof chemical residue in soil, dead seedling, rotten root, low atrophy, stiff seedling, yellow leaf, dry tip, imbalance in photosynthesis, dehydration, fertilizer removal and other variation symptoms in the seedling stage of crops. The additive of the invention is sprayed for 40 hours to basically recover normal growth.
Preferably, the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive consists of 0.01 to 3 weight percent of carbon-adsorbed 4-hydroxycoumarin and 97 to 99.99 weight percent of carbon-adsorbed polyglutamic acid. Preferably, the purity of the carbon-adsorbed 4-hydroxycoumarin is more than 99.8%.
In order to improve the purity of the 4-hydroxycoumarin, the carbon-adsorbed 4-hydroxycoumarin is preferably prepared by a method comprising the following steps: 1) dissolving 4-hydroxycoumarin in solvent, adding biochar, and heating and stirring at 35-80 deg.C for 6-12 hr; the mass ratio of the biochar to the 4-hydroxycoumarin is 1: 15-25; 1-2L of solvent is corresponding to each mol of 4-hydroxycoumarin;
2) heating and stirring in the step 1), filtering, removing residual solid in the filtrate, and dissolving in water, wherein each mol of 4-hydroxycoumarin corresponds to 0.75-2L of water; heating to 65-75 deg.C, separating the upper oil layer, and adjusting pH to 5.5-6.5 with sulfuric acid; then reducing the liquid temperature to 0-4 ℃ to ensure that the 4-hydroxycoumarin is completely separated out; filtering, washing with water until the washing liquid is neutral, and drying the filter cake to obtain the finished product of the carbon-adsorbed 4-hydroxycoumarin.
Preferably, the solvent in step 1) is 30% ethanol aqueous solution or water.
Preferably, the mass ratio of the biochar to the 4-hydroxycoumarin in the step 1) is 1: 20.
preferably, the temperature of the liquid is reduced in step 2) by adding ice.
Preferably, step 1) corresponds to 1.5L of solvent per mol of 4-hydroxycoumarin.
Preferably, in step 2) 0.75L of water is used per mol of 4-hydroxycoumarin.
The application of the carbon-adsorption 4-hydroxycoumarin herbicide safety additive in treatment of the side effects of the herbicide is characterized in that the carbon-adsorption 4-hydroxycoumarin herbicide safety additive is used for degrading the herbicide in soil, the dosage of the carbon-adsorption 4-hydroxycoumarin herbicide safety additive is 40-120 g/mu, and the carbon-adsorption 4-hydroxycoumarin herbicide safety additive is composed of 0.001-5 wt% of carbon-adsorption 4-hydroxycoumarin and 95-99.999 wt% of carbon-adsorption polyglutamic acid.
The carbon adsorption 4-hydroxycoumarin herbicide safety additive can be used for removing herbicide phytotoxicity. Specifically, the carbon adsorption 4-hydroxycoumarin herbicide safety additive can be independently used for removing herbicide phytotoxicity, and the use amount of the carbon adsorption 4-hydroxycoumarin herbicide safety additive in the removal of herbicide phytotoxicity is 1100-1300g/hm2. In particular, the followingThe carbon adsorption 4-hydroxycoumarin herbicide safety additive can be used together with a herbicide, and when the carbon adsorption 4-hydroxycoumarin herbicide safety additive is used together with the herbicide, the using amount of the carbon adsorption 4-hydroxycoumarin herbicide safety additive is 40-120 g/mu.
The carbon adsorption 4-hydroxycoumarin herbicide safety additive can accelerate the residue decomposition of the herbicide after use and improve the efficacy of the herbicide; the invention can eliminate a plurality of diseases caused by hidden phytotoxicity of the herbicide; the influence of herbicide residue on the next-stubble crops is solved, and the phenomena of dead seedlings, yellow seedlings, dead seedlings, withered seedlings, leaf spots, photosynthesis disorder, dehydration, fertilizer removal and the like are eliminated; meanwhile, the health of human body can be improved, the harm of herbicide residue to human is reduced, and the occurrence of cardiovascular and cerebrovascular diseases and other diseases is reduced. The large-area experiment proves that the carbon adsorption 4-hydroxycoumarin herbicide safety additive has good product effect and obvious yield increasing effect.
Preferably, the herbicide is one or more of tribenuron-methyl, chlorimuron-ethyl, marshall butachlor, bensulfuron-methyl, pyrazosulfuron-ethyl, prometryn and simetryn. The carbon adsorption 4-hydroxycoumarin herbicide safety additive of the invention can accelerate the residual decomposition of the herbicide after use.
More preferably, the herbicide is tribenuron-methyl wettable powder, wherein the effective mass of the tribenuron-methyl is 10%. In actual use, the dosage of tribenuron-methyl wettable powder of which the effective mass is 10 percent per mu is 10g per mu, and 40g of the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive is used.
More preferably, the herbicide is a marshall butachlor emulsion with an effective mass of marshall butachlor of 60%. When the herbicide is actually used, the dosage of each mu is 100mL of 60 percent Marshall butachlor emulsifiable concentrate, and 40g of the safe additive of the 4-hydroxycoumarin herbicide is adsorbed by carbon.
Preferably, the carbon-adsorbed 4-hydroxycoumarin is prepared by a method comprising the following steps:
1) dissolving 4-hydroxycoumarin in solvent, adding biochar, and heating and stirring at 35-80 deg.C for 6-12 hr; the mass ratio of the biochar to the 4-hydroxycoumarin is 1: 15-25; 1-2L of solvent is corresponding to each mol of 4-hydroxycoumarin;
2) heating and stirring in the step 1), filtering, removing residual solid in the filtrate, and dissolving in water, wherein each mol of 4-hydroxycoumarin corresponds to 0.75-2L of water; heating to 65-75 deg.C, separating the upper oil layer, and adjusting pH to 5.5-6.5 with sulfuric acid; then reducing the liquid temperature to 0-4 ℃ to ensure that the 4-hydroxycoumarin is completely separated out; filtering, washing with water until the washing liquid is neutral, and drying the filter cake to obtain the finished product of the carbon-adsorbed 4-hydroxycoumarin.
Preferably, the solvent in step 1) is 30% ethanol aqueous solution or water.
Preferably, the mass ratio of the biochar to the 4-hydroxycoumarin in the step 1) is 1: 20.
preferably, the temperature of the liquid is reduced in step 2) by adding ice.
Preferably, step 1) corresponds to 1.5L of solvent per mol of 4-hydroxycoumarin.
Preferably, in step 2) 0.75L of water is used per mol of 4-hydroxycoumarin.
Drawings
FIG. 1 is a liquid chromatogram of a chlorimuron-ethyl standard in test example 2 of the invention;
FIG. 2 is a liquid chromatogram of control detection of toxic soil without using a carbon-adsorbed 4-hydroxycoumarin herbicide safety additive in test example 2 of the present invention;
FIG. 3 is a liquid chromatogram of soil sample detection using carbon-adsorbed 4-hydroxycoumarin herbicide safety additive in test example 2 of the present invention;
FIG. 4 is a graph showing the change in the number of stalks per hole of rice investigated in test example 3 of the present invention;
FIG. 5 is a graph showing the comparison of phytotoxicity and control of paddy field in test example 4 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The equipment and reagents used in the examples and the experimental examples were commercially available except as specifically indicated. The tribenuron-methyl wettable powder used in the following examples and test examples has an effective tribenuron-methyl mass of 10%. The carbon-adsorbed polyglutamic acid can be prepared by the method disclosed in the patent with the application number of 201410284757.8.
Example 1 of a carbon-adsorbed 4-hydroxycoumarin herbicide safety additive
The carbon adsorption 4-hydroxycoumarin herbicide safety additive in this example: consists of 0.1 percent of carbon-adsorbed 4-hydroxycoumarin and 99.9 percent of carbon-adsorbed polyglutamic acid in percentage by weight.
The carbon-adsorbed 4-hydroxycoumarin in the example was prepared by the following method:
1) dissolving 162.1g of 4-hydroxycoumarin in 1500mL of 30% ethanol solution, adding biochar, and heating and stirring at 70 ℃ for 10 hours; the mass ratio of the biochar to the 4-hydroxycoumarin is 1: 20;
2) heating and stirring in the step 1), filtering, removing residual solid in the filtrate, and dissolving in 0.75L of water; heating to 70 deg.C, separating the upper oil layer, and adjusting pH to 6.0 with sulfuric acid; then adding ice to completely separate out the 4-hydroxycoumarin; filtering, washing with water until the washing liquid is neutral, and drying the filter cake to obtain the finished product of the carbon-adsorbed 4-hydroxycoumarin.
The purity of 4-hydroxycoumarin in the obtained carbon-adsorbed 4-hydroxycoumarin is more than 99.8%.
Preferably, the carbon-adsorption 4-hydroxycoumarin herbicide safety additive in the embodiment is added together with the herbicide in the tillering stage before winter, 10g of tribenuron-methyl wettable powder (10% of tribenuron-methyl effective mass content) and 40g of carbon-adsorption 4-hydroxycoumarin herbicide safety additive are added in each mu of land.
Preferably, the carbon-adsorption 4-hydroxycoumarin herbicide safety additive in the embodiment is added together with the herbicide in the tillering stage before winter, 10g of tribenuron-methyl wettable powder (10% of tribenuron-methyl effective mass content) and 80g of carbon-adsorption 4-hydroxycoumarin herbicide safety additive are added in each mu of land.
Preferably, the carbon-adsorption 4-hydroxycoumarin herbicide safety additive in the embodiment is added together with the herbicide in the tillering stage before winter, 10g of tribenuron-methyl wettable powder (10% of tribenuron-methyl effective mass content) and 120g of carbon-adsorption 4-hydroxycoumarin herbicide safety additive are added in each mu of land.
Preferably, the carbon-adsorption 4-hydroxycoumarin herbicide safety additive in the embodiment is added together with the herbicide in the paddy field, 100mL of the marshall butachlor emulsifiable concentrate with the herbicide concentration of 60 percent is added in each mu of land, and 40g of the carbon-adsorption 4-hydroxycoumarin herbicide safety additive is added in each mu of land.
Example 2 of a carbon-adsorbed 4-hydroxycoumarin herbicide safety additive
The carbon adsorption 4-hydroxycoumarin herbicide safety additive in this example: consists of 0.01 percent of carbon-adsorbed 4-hydroxycoumarin and 99.99 percent of carbon-adsorbed polyglutamic acid in percentage by weight. The purity of the 4-hydroxycoumarin is more than 99.8%.
Example 3 of a carbon-adsorbed 4-hydroxycoumarin herbicide safety additive
The carbon adsorption 4-hydroxycoumarin herbicide safety additive in this example: consists of 3 percent of carbon-absorbed 4-hydroxycoumarin and 97 percent of carbon-absorbed polyglutamic acid in percentage by weight. The purity of the 4-hydroxycoumarin is more than 99.8%.
Example 1 use of a carbon-adsorbed 4-hydroxycoumarin herbicide safety additive to remediate herbicide hazards
In the embodiment, the application of the carbon-adsorbed 4-hydroxycoumarin in treatment of the side effect of the herbicide is that the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive is used for degrading the herbicide in soil, and the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive consists of 0.001-5 wt% of carbon-adsorbed 4-hydroxycoumarin and 95-99.999 wt% of carbon-adsorbed polyglutamic acid. The dosage of the carbon adsorption 4-hydroxycoumarin herbicide safety additive is 40-120 g/mu.
The carbon adsorption 4-hydroxycoumarin herbicide safety additive can be independently used for removing herbicide phytotoxicity, and the use amount of the carbon adsorption 4-hydroxycoumarin herbicide safety additive in the removal of herbicide phytotoxicity is 1100-1300g/hm2. In particular, the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive can be used with a herbicide, and when used with a herbicide, the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive is used with a herbicideThe using amount of the safe additive for adsorbing the 4-hydroxycoumarin herbicide is 40-120 g/mu; the chemical herbicide is one or more of tribenuron-methyl, chlorimuron-ethyl, marshall butachlor, bensulfuron-methyl, pyrazosulfuron-ethyl, prometryn and simetryn.
Test example 1 test for controlling side effects of herbicide in wheat field by using carbon-adsorbed 4-hydroxycoumarin herbicide safety additive
1. In this experimental example, the effect of controlling the side effect of a herbicide in a wheat field was studied with respect to a carbon-adsorbed 4-hydroxycoumarin herbicide safety additive (as shown in example 1 of the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive) composed of carbon-adsorbed 4-hydroxycoumarin and carbon-adsorbed polyglutamic acid. In order to verify the prevention and control effect and safety of the carbon adsorption 4-hydroxycoumarin herbicide safety additive on the side effect of the herbicide in the wheat field, experiments are carried out in a certain wheat field in Henan, and the experimental process and results are as follows.
2. Test conditions
2.1 test materials
The wheat variety is Bainong dwarf 58, and the herbicide is tribenuron-methyl wettable powder (the effective mass of tribenuron-methyl is 10%); a char-adsorbed 4-hydroxycoumarin herbicide safety additive (as shown in example 1 of the char-adsorbed 4-hydroxycoumarin herbicide safety additive), wherein the char-adsorbed 4-hydroxycoumarin content is 0.1%.
2.2 control of weeds
The weeds in the wheat field are mainly broadleaf weeds such as cleavers, descurainia sophia, shepherd's purse, speedwell, sun euphorbia herb, Li and the like, and grassy weeds such as wild oat, rhynchophylla and the like.
3. Design of experiments
TABLE 1 Experimental design of test agent for application before winter
4. Calculation method
The calculation formula of the weed control effect of the herbicide is as follows:
control effect (%) (% control zone weed plant number or fresh weight-treatment zone weed plant number or fresh weight)/control zone weed plant number or fresh weight × 100%.
The wheat yield calculation formula is as follows:
the yield (kg/mu) is equal to ear number per mu, ear number per mu and thousand kernel weight per mu.
5. Test results
TABLE 2 survey of growth of wheat treated differently after 120 days after application
As can be seen from Table 2, the tribenuron-methyl wettable powder (10 g/mu) is used for weeding in the tillering stage before winter, and the average single-plant fresh weight, tillering number and secondary root number of the wheat in the treatment area are all lower than those of the control, which shows that the tribenuron-methyl wettable powder is used for weeding and has certain side effect on the wheat; the tribenuron-methyl wettable powder and the carbon adsorption 4-hydroxycoumarin herbicide safety additive are mixed for use, so that the generation of the side effect of the tribenuron-methyl can be prevented, the growth of wheat is promoted, and the growth of plants is normal along with the increase of the use amount of the carbon adsorption 4-hydroxycoumarin herbicide safety additive.
TABLE 3 weed control efficacy of different treatments 150 days after application
As can be seen from Table 3, compared with the control, the control effect of each treatment on broadleaf weeds is obvious, which indicates that the weeding effect of tribenuron-methyl is not affected when the carbon adsorption 4-hydroxycoumarin herbicide safety additive is mixed with tribenuron-methyl wettable powder, and the carbon adsorption 4-hydroxycoumarin herbicide safety additive can be mixed with tribenuron-methyl wettable powder for use.
TABLE 4 yield results of different treatments
| Treatment of | Yield (kg) | Yield increase (%) |
| 1 | 495.56 | 1.33 |
| 2 | 523.94 | 7.14 |
| 3 | 550.06 | 12.48 |
| 4 | 491.39 | 0.48 |
| 5 | 489.04 | / |
As can be seen from Table 4, the yield of wheat can be increased by mixing the carbon adsorption 4-hydroxycoumarin herbicide safety additive with the tribenuron-methyl wettable powder, and the yield increase of a treatment area with 10g of tribenuron-methyl wettable powder and 120g of carbon adsorption 4-hydroxycoumarin herbicide safety additive per mu is the highest and reaches 12.48 percent; the tribenuron-methyl wettable powder is used alone, and the yield increasing effect is not obvious.
6. Conclusion of the experiment
After the carbon-adsorption 4-hydroxycoumarin herbicide safety additive is mixed with the tribenuron-methyl wettable powder for use, the wheat grows normally, and dominant phytotoxicity symptoms such as withered leaves, malformation and yellowing do not appear, so that the carbon-adsorption 4-hydroxycoumarin herbicide safety additive is safe to the wheat, and the carbon-adsorption 4-hydroxycoumarin herbicide safety additive is mixed with the tribenuron-methyl wettable powder to prevent the occurrence of side effects of the herbicide; from comprehensive evaluation of the weeding effect of the mixture of the carbon adsorption 4-hydroxycoumarin herbicide safety additive and tribenuron-methyl wettable powder, the safety and yield increasing effect of wheat and the like, the mixture of the carbon adsorption 4-hydroxycoumarin herbicide safety additive and the herbicide can effectively prevent the side effect of the herbicide, remarkably improve the yield of wheat, be widely popularized and applied in wheat production and be suitable for using 80g of the carbon adsorption 4-hydroxycoumarin herbicide safety additive per mu.
Test example 2 test for degrading residual herbicide in soil by using carbon-adsorbed 4-hydroxycoumarin herbicide safety additive
Heilongjiang is a big province in crop planting in China, and the problem of herbicide residue in soil is caused by using a large amount of herbicide, so that the yield and the quality of crops are seriously influenced. To solve the problem, the applicant carried out herbicide residue detection on a soybean field in Heilongjiang using a carbon-adsorbed 4-hydroxycoumarin herbicide safety additive (as shown in example 1 of the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive) and a soybean field without using the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive. The detection conditions were as follows:
1. soil collection: collecting toxic soil without using carbon to adsorb 4-hydroxycoumarin herbicide safety additive: the collection place is a control soybean field without using the carbon adsorption 4-hydroxycoumarin herbicide safety additive in a certain place of Heilongjiang, and the drug use condition is 130-2(this herbicide has been in use for more than 3 years).
Soil sample collection using carbon-adsorbed 4-hydroxycoumarin herbicide safety additives: the control soybean field which is collected in a certain place of Heilongjiang and uses the carbon adsorption 4-hydroxycoumarin herbicide safety additive is used for treating the soil once by using the carbon adsorption 4-hydroxycoumarin herbicide safety additive, and the dosage of the carbon adsorption 4-hydroxycoumarin herbicide safety additive is 1200g/hm2The application method is that the fertilizer is uniformly sprayed to soil.
2. Soil treatment and detection:
weighing 10g of air-dried soil sample, soaking the air-dried soil sample in 15mL of acetonitrile/water (8:2), oscillating for 35min for extraction, carrying out vacuum filtration, transferring the filtrate into a separating funnel, adding 10mL of 0.1mol/L calcium chloride aqueous solution, extracting for 3 times by using dichloromethane, and carrying out rotary evaporation at 35 ℃ and reduced pressure concentration until the volume is approximate to the measured volume. The concentrate was filtered through a 0.45 μm membrane and analyzed by high performance liquid chromatography.
A liquid chromatogram of a chlorimuron-ethyl standard product is shown in figure 1, a poison soil contrast detection liquid chromatogram of a 4-hydroxycoumarin herbicide safety additive which is not adsorbed by carbon is shown in figure 2, and a soil sample detection liquid chromatogram of the 4-hydroxycoumarin herbicide safety additive which is adsorbed by carbon is shown in figure 3; the soil test data are shown in table 5, wherein a represents the average value of chlorimuron-ethyl, and C represents the concentration (μ g/L) of chlorimuron-ethyl; the result shows that compared with the soil sample which does not use the carbon adsorption 4-hydroxycoumarin herbicide safety additive, the content of chlorimuron-ethyl in the soil sample after the carbon adsorption 4-hydroxycoumarin herbicide safety additive is not detected.
TABLE 5 residual effect of carbon adsorption of 4-hydroxycoumarin herbicide safety additive on herbicide degradation
Test example 3 demonstration of a carbon-adsorbed 4-hydroxycoumarin herbicide safety additive
1. Test demonstration sites: a test area base of Heilongjiang.
2. The purpose of the test is as follows: the prevention and control and the alleviation effects of the side effects of the carbon adsorption 4-hydroxycoumarin herbicide safety additive are investigated and verified, and meanwhile, the safety and the side effects of the currently applied herbicide, the safety and the side effects of the carbon adsorption 4-hydroxycoumarin herbicide safety additive (as shown in example 1 of the carbon adsorption 4-hydroxycoumarin herbicide safety additive), the appropriate use period and the appropriate use amount of the carbon adsorption 4-hydroxycoumarin herbicide safety additive and other matching technologies are discussed. Cell experiments, requiring 4 replicates.
3. The test treatment method comprises the following steps:
a. artificial weeding: therein is retained 5m2No weed was removed (treatment code a).
b. Two times of herbicide application: the herbicide formula is shown in table 6 after local conventional treatment (5-7 days before the transplanting and 10-15 days after the transplanting).
c. On the basis of the treatment b, 40 g/mu of the 4-hydroxycoumarin herbicide safety additive is added in the herbicide used twice.
d. On the basis of the treatment b, the herbicide is used twice, and 40 g/mu of the safe additive of the 4-hydroxycoumarin herbicide is added in the previous time by carbon adsorption.
e. On the basis of the treatment b, the herbicide is used twice, and 40 g/mu of the 4-hydroxycoumarin herbicide safety additive is added for carbon adsorption at the later time.
f. Artificial weeding is carried out, and after 10-15 days of seedling transplanting, 40 g/mu of carbon adsorption 4-hydroxycoumarin herbicide safety additive (without herbicide) is sprayed.
TABLE 6 herbicide formula and soil condition in Heilongjiang certain Rice test area
4. And (3) test results:
the investigation results of the test are: before the rice transplanting, the rice transplanting shows phytotoxicity symptoms 3 days after the rice transplanting. The rate of the plant suffering from phytotoxicity is investigated in 5 months and 22 days: the heaviest phytotoxicity of treatment b (two times with herbicide) was 6.1%, and the lightest phytotoxicity of treatment d (on the basis of treatment b, the former carbon adsorption of 4-hydroxycoumarin herbicide safety additive) was 3.4%. Treatment b and treatment e were more phytotoxic in terms of leaf color (as shown in Table 7).
TABLE 7 investigation of safety of herbicide applied to certain Rice test areas in Heilongjiang
Note: the phytotoxicity condition is divided into: none, slight, heavy, severe; the color of the leaves can be normal, light yellow, brown or other; the difference in plant height of rice was compared to the treatment plot A.
The results show that: the carbon adsorption 4-hydroxycoumarin herbicide safety additive can reduce the occurrence degree of rice phytotoxicity when being mixed with herbicide for application. The phytotoxicity rate can be reduced by 1/3-1/2. The dry and fresh weight of the rice is investigated 1 day before and 20 days after the application of the stem and leaf treatment herbicide, and the treatment by adding the carbon adsorption 4-hydroxycoumarin herbicide safety additive is increased compared with the treatment by only using the herbicide, which shows that the carbon adsorption 4-hydroxycoumarin herbicide safety additive has a relieving effect on the phytotoxicity of the herbicide (as shown in tables 8 and 9).
TABLE 8 Rice growth status survey on 6 months and 8 days in Heilongjiang certain Rice test area
| d | 20.6 | 0.079 | 0.052 | 0.131 | 0.049 | 0.014 | 0.063 |
| e | 22.1 | 0.085 | 0.037 | 0.122 | 0.051 | 0.009 | 0.06 |
| f | 23.1 | 0.091 | 0.051 | 0.142 | 0.054 | 0.015 | 0.069 |
TABLE 9 investigation of Rice growth status in Heilongjiang A Rice test area on 6 months and 29 days
The stem number of the carbon adsorption 4-hydroxycoumarin herbicide safety additive to each hole of rice is adjusted, and the result is shown in figure 4, and the result shows that the carbon adsorption 4-hydroxycoumarin herbicide safety additive can relieve the inhibition effect of the herbicide on rice tillering and increase the stem number. The stem number of each hole is not greatly different in each treatment of 15 days in 6 months and 21 days in 6 months; the difference between treatments is obvious at 29 days after 6 months, and the number of the treatment sites arranged at the first 3 positions is 22, 20.5 and 20.1 for f (artificial weeding and 1 carbon adsorption of 4-hydroxycoumarin herbicide safety additive), d (2 times weeding and the previous carbon adsorption of 4-hydroxycoumarin herbicide safety additive) and e (2 times weeding and the next carbon adsorption of 4-hydroxycoumarin herbicide safety additive), and is increased by 15.1%, 7.3% and 5.2% compared with b. In 14 days in 7 months, the stems of each hole are arranged at the first 3 positions of a (artificial weeding), c (2 times of weeding and 2 times of adding the charcoal adsorption 4-hydroxycoumarin herbicide safety additive) and f (artificial weeding and 1 time of charcoal adsorption 4-hydroxycoumarin herbicide safety additive) are respectively 22, 20.8 and 20.0, and are respectively increased by 30.9 percent, 23.8 percent and 19.0 percent compared with b.
The rice to be tested was analyzed in the test area of rice in Heilongjiang (see Table 10). The analysis shows that the protein content and the amylose content of the treatment b (two single herbicides) are reduced to different degrees compared with the treatment a (artificial weeding). Compared with the protein content of b, the processing ratio of the carbon adsorption 4-hydroxycoumarin herbicide safety additive is improved by more than 0.5%, the amylose content is improved by more than 0.6%, and meanwhile, the normal grain ratio is improved, the broken grain rate is reduced, and the colored grain rate is reduced. Wherein the protein and amylose content of f (artificial weeding, foliage spraying charcoal adsorption 4-hydroxycoumarin herbicide safety additive) is highest. The herbicide has certain influence on rice quality, and the carbon adsorption 4-hydroxycoumarin herbicide safety additive has the effects of reducing the influence and improving the rice quality.
TABLE 10 Rice quality analysis Table for applying carbon adsorption 4-hydroxycoumarin herbicide safety additive to rice in certain Heilongjiang rice test area
5. And (4) test conclusion: the carbon adsorption 4-hydroxycoumarin herbicide safety additive is safe and harmless to the growth and development of crops, can promote the growth and development of crops after being used, enhances the drug resistance of the crops, is used in combination with the herbicide, has no side effects of reducing the weeding effect and the like, and is a harmonious partner of the herbicide; the carbon adsorption 4-hydroxycoumarin herbicide safety additive has the effects of reducing and relieving the side effects of the herbicide, can effectively shorten the inhibition period of the herbicide on the growth of crops, improve the yield and improve the product quality; the application technology of the carbon adsorption 4-hydroxycoumarin herbicide safety additive is an advanced green agricultural technology for implementing crop safety stubble changing and supporting crop structure adjustment.
Test example 4 case 1 of phytotoxicity relief of carbon-adsorbed 4-hydroxycoumarin herbicide safety additive
The rice is mainly planted in Heilongjiang, the yield per unit and the total yield are in the international leading level, herbicide phytotoxicity frequently occurs along with the excessive use of the herbicide and the mixed use of different herbicides, serious herbicide phytotoxicity is caused by the mixed use of the herbicide in Heilongjiang in 2017 in 6 months, and the phytotoxicity is successfully removed by the treatment of the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive. The specific situation is as follows:
the rice phytotoxicity condition: a place: somewhere in Heilongjiang; the administration time is as follows: 6 months and 5 days in 2017; the pesticide name is as follows: mefenacet, bensulfuron-methyl, pyrazosulfuron-ethyl, prometryn and simetryn; the usage method comprises the following steps: after the 5 herbicides are mixed, the mixture is mixed with water according to the recommended dose and then directly thrown and applied to the paddy field. The phytotoxicity time is as follows: 6, 8 and 6 months in 2017, large-area phytotoxicity appears, all rice seedlings wither and fall down, and the rice seedlings are dead in production if not treated.
Carbon-adsorbed 4-hydroxycoumarin herbicide safety additive (as shown in example 1 of carbon-adsorbed 4-hydroxycoumarin herbicide safety additive) rescue time: 6 months and 8 days in 2017; the method for remedying the carbon adsorption 4-hydroxycoumarin herbicide safety additive comprises the following steps: use charcoal adsorption 4-hydroxy coumarin herbicide safety additive 1200g/hm2And after being mixed with water, the leaf surface is uniformly sprayed. And (3) eliminating phytotoxicity: in 2017, 6, 15, the result of using the carbon to adsorb the 4-hydroxycoumarin herbicide safety additive is shown in fig. 5, wherein A is a rice phytotoxicity graph; b is a graph of treating rice by using the carbon adsorption 4-hydroxycoumarin herbicide safety additive; the results show that the phytotoxicity of the rice is completely relieved, the rice grows well, and the loss is saved for farmers.
Claims (10)
1. A carbon adsorption 4-hydroxycoumarin herbicide safety additive is characterized in that: consists of 0.001 to 5 weight percent of carbon-adsorbed 4-hydroxycoumarin and 95 to 99.999 weight percent of carbon-adsorbed polyglutamic acid;
the dosage of the carbon adsorption 4-hydroxy coumarin herbicide safety additive is 40-120 g/mu.
2. The carbon-adsorbed 4-hydroxycoumarin herbicide safety additive of claim 1, wherein: consists of 0.01 to 3 weight percent of carbon-adsorbed 4-hydroxycoumarin and 97 to 99.99 weight percent of carbon-adsorbed polyglutamic acid.
3. The carbon-adsorbed 4-hydroxycoumarin herbicide safety additive of claim 1, wherein: the carbon-adsorbed 4-hydroxycoumarin is prepared by a method comprising the following steps:
1) dissolving 4-hydroxycoumarin in solvent, adding biochar, and heating and stirring at 35-80 deg.C for 6-12 hr; the mass ratio of the biochar to the 4-hydroxycoumarin is 1: 15-25; 1-2L of solvent is corresponding to each mol of 4-hydroxycoumarin;
2) heating and stirring in the step 1), filtering, removing residual solid in the filtrate, and dissolving in water, wherein each mol of 4-hydroxycoumarin corresponds to 0.75-2L of water; heating to 65-75 deg.C, separating the upper oil layer, and adjusting pH to 5.5-6.5 with sulfuric acid; then reducing the liquid temperature to 0-4 ℃ to ensure that the 4-hydroxycoumarin is completely separated out; filtering, washing with water until the washing liquid is neutral, and drying the filter cake to obtain the finished product of the carbon-adsorbed 4-hydroxycoumarin.
4. The carbon-adsorbed 4-hydroxycoumarin herbicide safety additive of claim 3, wherein: the solvent in the step 1) is 30% ethanol water solution or water.
5. The carbon-adsorbed 4-hydroxycoumarin herbicide safety additive of claim 3, wherein: the mass ratio of the biochar to the 4-hydroxycoumarin in the step 1) is 1: 20.
6. the carbon-adsorbed 4-hydroxycoumarin herbicide safety additive of claim 3, wherein: and in the step 2), the temperature of the liquid is reduced by using an ice adding mode.
7. The carbon-adsorbed 4-hydroxycoumarin herbicide safety additive of claim 3, wherein: step 1) 1.5L of solvent for each mol of 4-hydroxycoumarin.
8. The carbon-adsorbed 4-hydroxycoumarin herbicide safety additive of claim 7, wherein: in step 2), each mol of 4-hydroxycoumarin corresponds to 0.75L of water.
9. The application of the carbon adsorption 4-hydroxycoumarin in the treatment of the side effect of the herbicide is characterized in that: the method is characterized in that a carbon adsorption 4-hydroxycoumarin herbicide safety additive is used for degrading herbicides in soil, the using amount of the carbon adsorption 4-hydroxycoumarin herbicide safety additive is 40-120 g/mu, and the carbon adsorption 4-hydroxycoumarin herbicide safety additive is composed of 0.001-5 wt% of carbon adsorption 4-hydroxycoumarin and 95-99.999 wt% of carbon adsorption polyglutamic acid.
10. The use of carbon-adsorbed 4-hydroxycoumarin as claimed in claim 9 in the management of herbicide side effects, wherein: the herbicide is one or more of tribenuron-methyl, acetochlor, nicosulfuron, atrazine, 2.4 d isooctyl ester, fomesafen, mesotrione, quizalofop-p-ethyl, marshall butachlor, bensulfuron-methyl, pyrazosulfuron-ethyl and fluoroglycofen-ethyl.
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