CN108522564A - A kind of preparation method of rice herbicide - Google Patents

A kind of preparation method of rice herbicide Download PDF

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CN108522564A
CN108522564A CN201810463129.4A CN201810463129A CN108522564A CN 108522564 A CN108522564 A CN 108522564A CN 201810463129 A CN201810463129 A CN 201810463129A CN 108522564 A CN108522564 A CN 108522564A
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take
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何治伟
庄文琴
刘红妹
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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
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • 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
    • A01N37/02—Saturated carboxylic acids or thio analogues thereof; Derivatives thereof
    • 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
    • A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/22—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom rings with more than six members
    • 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
    • A01N61/00—Biocides, pest repellants or attractants, or plant growth regulators containing substances of unknown or undetermined composition, e.g. substances characterised only by the mode of action
    • 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
    • A01N63/00—Biocides, pest repellants or attractants, or plant growth regulators containing microorganisms, viruses, microbial fungi, animals or substances produced by, or obtained from, microorganisms, viruses, microbial fungi or animals, e.g. enzymes or fermentates
    • 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
    • A01N63/00—Biocides, pest repellants or attractants, or plant growth regulators containing microorganisms, viruses, microbial fungi, animals or substances produced by, or obtained from, microorganisms, viruses, microbial fungi or animals, e.g. enzymes or fermentates
    • A01N63/30—Microbial fungi; Substances produced thereby or obtained therefrom
    • 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
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/40—Liliopsida [monocotyledons]
    • A01N65/44—Poaceae or Gramineae [Grass family], e.g. bamboo, lemon grass or citronella grass

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Plant Pathology (AREA)
  • Wood Science & Technology (AREA)
  • Environmental Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Microbiology (AREA)
  • Biotechnology (AREA)
  • Mycology (AREA)
  • Virology (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a kind of preparation methods of rice herbicide, belong to pesticide field.The present invention is using aniline and bromine as raw material; bromo-reaction occurs; reaction product is as an active substructure; concentrated nitric acid is added to be nitrified; using benzene oxygen acetyl group as another active substructure; using ethyl acetate as solvent; addition triethylamine is acid binding agent; it reacts with aryloxyacetic acid, thionyl chloride etc., obtains herbicidal active compounds, herbicidal active compounds can inhibit the synthesis of lipid in plant; influence the proteinase activity of weeds chitting piece; to destroy its synthesis, the germinating growth process of weeds is hindered, achievees the purpose that kill weeds.The present invention solves current herbicide and is not thorough to weed eradication, also easily leads to the problem of resistance weed enhances.

Description

A kind of preparation method of rice herbicide
Technical field
The invention belongs to pesticide fields, and in particular to a kind of preparation method of rice herbicide.
Background technology
Rice belongs to most important one one kind in cereal crops, but efficient and green control is needed to have in production The case where doing harm to biology, preventing it from leading to grain drop in production.Rice underproduction many factors are caused to be no more than weeds in weeds in paddy field, currently It takes the mode of chemical weed control to become common mode, and occurs a variety of weeds in rice terrace by developing corresponding weeding Agent and effectively control influence of the weeds to rice terrace.The difference of combining form is analyzed, and the weeds in rice field can divide It is following several：The first is the leaf weeds of list, and second is dicots weeds, and the weeds of grass family and Cyperaceae It is then monocotyledonous weeds, broad leaved weed is then dicots weeds, and different remove is selected with reference to the type that this weeds divides Careless agent brings certain reference value.By development for many years, the kind that can be used for herbicide in rice field and number Amount all with day increase severely, including type have：Amides, diphenyl ether, bipyridyliums, sulfonamides, Tetrazoline series, carboxylate Class, quinoline carboxylic acid, organic phosphates, sulfonylurea and heterocyclic.And it is miscellaneous to be then divided into broad-leaved with reference to the target of management of weeds Grass, grassy weed, sedge weed and broad spectrum activity herbicide.
Chemical pesticide is the important leverage of modern agriculture good harvest, and wherein herbicide is pesticide producing and the maximum composition used Part.Although herbicide it is long-term, a large amount of, be widely used and promote Food Production, current herbicide is not thorough to weed eradication Bottom also easily leads to resistance weed enhancing.Therefore, producing a kind of efficient rice herbicide has prodigious market prospects.
Invention content
The technical problems to be solved by the invention：Weed eradication is not thorough for current herbicide, also easily leads to weeds Drug resistance enhancing the problem of, a kind of preparation method of rice herbicide is provided.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of rice herbicide, which is characterized in that the preparation method includes the following steps：
（1）Take aniline in mass ratio 1：25 are added aqueous solution of hydrogen bromide, obtain mixed liquor A, take bromine in mass ratio 1：8 are added bromination Aqueous solution of hydrogen obtains mixed liquid B, takes mixed liquid B in mass ratio 3：5 are added dropwise to mixed liquor A, control 25 ~ 30min of time for adding, in 20 ~ 25 DEG C are stirred, and are evaporated under reduced pressure, and filter, and take and filter slag through distilling water washing, obtain washings；
（2）Take washings in mass ratio 1：10 be added glacial acetic acids, be stirred in 20 ~ 25 DEG C, add glacial acetic acid quality 10 ~ 15% nitric acid, is stirred, and obtains stirring mixture, takes stirring mixture in mass ratio 10：1：3 are added acetic anhydride, glacial acetic acid, In 25 ~ 30 DEG C of heat preservations, mixture is obtained, mixture in mass ratio 1 is taken：100 are added 0 ~ 2 DEG C of distilled water, stand, vacuum distillation, Take precipitation；
（3）Take precipitation in mass ratio 2：It is stirred in 1 addition sodium bicarbonate solution, filters, take filter residue, take aryloxyacetic acid by matter Measure ratio 5：100：2 are added dichloromethane, thionyl chloride, and in 75 ~ 80 DEG C of back flow reactions, vacuum distillation must be evaporated under reduced pressure object a, take Filter residue in mass ratio 1：40 are added ethyl acetate, are stirred in 20 ~ 25 DEG C, add the triethylamine of filter residue quality 85 ~ 95%, It is stirred, obtains mixture a, take mixture a in mass ratio 3：2：10 are added vacuum distillation object a, ethyl acetate, are stirred in 2 ~ 4 DEG C Reaction is mixed, is filtered, is taken filtrate rotary evaporation, obtain rotary evaporation object, it is spare；
（4）Take dregs of beans in mass ratio 1：3：10 are added rice chaff, deionized water mixing, are stirred, obtain mixture, add mixing The alkali protease of amount of substance 1.5 ~ 3% obtains zymolyte, takes zymolyte in mass ratio 5 in 55 ~ 60 DEG C of enzymolysis：1 addition ammonium hydroxide stirs Mixing is mixed, enzyme deactivation filters, takes smoke filtrate to concentrate, obtain concentrate；
（5）It takes candida utili bacterium to be seeded in seed activation culture medium by 2% inoculum concentration, in 25 ~ 30 DEG C of cultures, obtains work Change culture and takes 400 ~ 500 parts of concentrates, 45 ~ 50 parts of activation culture objects, 0.2 ~ 0.4 part of phytase, 250 according to the mass fraction ~ 300 parts of water mixing obtain fermentate in 35 ~ 45 DEG C of fermentations, dry, obtain dried object；
（6）According to the mass fraction, 40 ~ 50 parts of sec-Butyl Acetates, 3 ~ 6 parts of brassin lactones, 15 ~ 20 parts of steps are taken（3）Spare Rotary evaporation object, 60 ~ 70 parts of dried objects, 4 ~ 7 parts of mixed extracts, 12 ~ 15 parts of hydroxypropyl-β-cyclodextrins, 60 ~ 80 parts of water are mixed It closes, is stirred in 80 ~ 85 DEG C, dry, pulverize sieving, collect sieving particle, obtain rice herbicide.
The step（5）Middle seed activation culture medium：According to the mass fraction, take 10 ~ 15 parts of yeast extracts, 15 ~ 20 parts Peptone, 18 ~ 20 parts of glucose, adjust pH to 6.0,121 DEG C of high pressure sterilization 20min to get.
The step（6）Middle mixed extracts：Take Chinese prickly ash, Rhizoma Et Radix Notopterygii in mass ratio 1：2：10 are added ethanol solution, through dioxy Change carbon supercritical extract, in 40 ~ 45 DEG C, 30MPa, CO2Flow is 15L/h, extracts 1 ~ 2h, obtains mixed extracts.
Compared with other methods, advantageous effects are the present invention：
（1）Using aniline and bromine as raw material bromo-reaction occurs for the present invention, reaction product is as an active substructure, then adds Enter concentrated nitric acid to be nitrified, triethylamine is added using ethyl acetate as solvent using benzene oxygen acetyl group as another active substructure It for acid binding agent, reacts with aryloxyacetic acid, thionyl chloride etc., obtains herbicidal active compounds, there is preferable selectivity, higher Drug effect, and medicament is easy to be degraded in plant, smaller to the harm of mammal, is inhaled by the young shoot of weeds and root It receives, the biosynthesis of fat and aliphatic acid is the necessary of maintenance weed growth body normal physiological function, and herbicidal active compounds can To inhibit the synthesis of lipid in plant, the proteinase activity of weeds chitting piece is influenced, to destroy its synthesis, hinders weeds Germinating growth process, achieve the purpose that kill weeds；
（2）The present invention is using rice chaff and dregs of beans as raw material, and containing a large amount of starch and crude protein, alkali protease enzymolysis is first added, Fermentation pretreatment is carried out to dregs of beans, rice chaff with candida utili, higher temperature condition is provided to phytase, then it is more advantageous It plays a role in phytase, promotes the dissolution of the nutriments such as organic acid and protein in rice chaff and dregs of beans, product is applied Paddy field surface, nutritional ingredient are easily that Institute of Micro-biology decomposes, and generate great amount of carbon dioxide and consume a large amount of oxygen in water, make water Rice is in strong reducing condition, and carbon dioxide increases therebetween, can hinder the root of hair and its growth and development of weeds, the extreme of oxygen The sprouting of grass-seed can be hindered by reducing, thus is kept weeds heavily suppressed or be choked to death, the organic acid of generation, inhibit weeds hair Root, germination, and can the calcination weeds tip of a root, lobus cardiacus, strong reduction reaction and organic acid can make the germination of weeds, root of hair by serious Inhibit, the pigment of organic acid and microorganism decomposition generation, the structural constituent of raw material are combined with soil colloid, and Soil surface water can be made muddy Turbid poor transparency, thus the photosynthesis of weeds is made to be obstructed, to inhibit weed growth, the method using biology is preferably prevented The recurrence for having stopped weeds plays mitigation to the anti-medicine dependence of herbicide, while the organic matters such as its organic acid generated carry The high activity of paddy soil, have stimulated the growth regulating of rice, improves the yield of rice；
（3）The present invention adds Chinese prickly ash, Rhizoma Et Radix Notopterygii extract, and it is amides active matter to have the functional mass of detoxication in Chinese prickly ash ingredient Matter is made of fatty acid part and amino part, and there are a large amount of coumarin kind compounds, the two to have higher work in Rhizoma Et Radix Notopterygii Property, when herbicidal active compounds enter in rice cell after addition, improves GSTs enzymatics and substitution reaction occurs into knot with GSH Object is closed, then is transported in central vacuole through correlation ABCC transporters on tonoplast, is decomposed accordingly in vacuole again later Metabolism is finally reached detoxication, rice root vigor is improved, with potential harmful substance around antagonism The Rhizosphere of Rice.
Specific implementation mode
A kind of preparation method of rice herbicide, includes the following steps：
Rice chaff：80 mesh are purchased from Huaiyuan County Wen Bo rice chaff processing factory.Dregs of beans：100 mesh are purchased from Shenzhen Hua Bao feed corporation,Ltds.
Seed activation culture medium：According to the mass fraction, take 10 ~ 15 parts of yeast extracts, 15 ~ 20 parts of peptones, 18 ~ 20 parts Glucose, adjust pH to 6.0,121 DEG C of high pressure sterilization 20min to get.
Mixed extracts：Take Chinese prickly ash, Rhizoma Et Radix Notopterygii in mass ratio 1：2：10 are added the ethanol solution that mass fraction is 80%, through two Carbonoxide supercritical extract, in 40 ~ 45 DEG C, 30MPa, CO2Flow is 15L/h, extracts 1 ~ 2h, obtains mixed extracts.
（1）Take aniline in mass ratio 1：25 are added the aqueous solution of hydrogen bromide that mass fraction is 10%, obtain mixed liquor A, take bromine In mass ratio 1：8 are added the aqueous solution of hydrogen bromide that mass fraction is 10%, obtain mixed liquid B, take mixed liquid B in mass ratio 3：5 are added dropwise To mixed liquor A, 25 ~ 30min of time for adding is controlled, 30 ~ 40min is stirred in 20 ~ 25 DEG C, be evaporated under reduced pressure, filtered, take suction filtration Slag obtains washings through distilling water washing；
（2）Take washings in mass ratio 1：10 are added glacial acetic acid, are stirred 15 ~ 20min in 20 ~ 25 DEG C, add glacial acetic acid The mass fraction of quality 10 ~ 15% be 98% nitric acid, be stirred 20 ~ 30min, obtain stirring mixture, take stirring mixture by Mass ratio 10：1：3 are added acetic anhydride, glacial acetic acid, keep the temperature 1 ~ 2h in 25 ~ 30 DEG C, obtain mixture, take mixture in mass ratio 1： 100 are added 0 ~ 2 DEG C of distilled water, stand 2 ~ 3h, and vacuum distillation takes precipitation；
（3）Take precipitation in mass ratio 2：It is stirred 1 ~ 2h in the sodium bicarbonate solution that 1 addition mass fraction is 5%, filters, takes Filter residue takes aryloxyacetic acid in mass ratio 5：100：2 addition dichloromethane, thionyl chloride subtract in 75 ~ 80 DEG C of 5 ~ 6h of back flow reaction Pressure distillation, must be evaporated under reduced pressure object a, take filter residue in mass ratio 1：40 are added ethyl acetate, it is stirred 20 in 20 ~ 25 DEG C ~ 30min adds the triethylamine of filter residue quality 85 ~ 95%, is stirred 5 ~ 10min, obtains mixture a, takes mixture a by quality Than 3：2：10 are added vacuum distillation object a, ethyl acetate, are stirred to react 3 ~ 4h in 2 ~ 4 DEG C, filter, take filtrate rotary evaporation, must revolve Turn evaporant, it is spare；
（4）Take dregs of beans in mass ratio 1：3：10 are added rice chaff, deionized water mixing, are stirred 20 ~ 30min in 120rpm, obtain Mixture adds the alkali protease of mixture quality 1.5 ~ 3%, digests 5 ~ 6h in 55 ~ 60 DEG C, obtains zymolyte, take zymolyte In mass ratio 5：The ammonium hydroxide that 1 addition mass fraction is 10% is stirred, and enzyme deactivation filters, takes smoke filtrate to concentrate, obtain concentrate；
（5）Take candida utili bacterium to be seeded in seed activation culture medium by 2% inoculum concentration, in 25 ~ 30 DEG C cultivate 24 ~ 48h obtains activation culture object, according to the mass fraction, takes 400 ~ 500 parts of concentrates, 45 ~ 50 parts of activation culture objects, 0.2 ~ 0.4 part of plant Sour enzyme, 250 ~ 300 parts of water mixing, ferment 15 ~ 20h in 35 ~ 45 DEG C, obtains fermentate, dry, obtains dried object；
（6）According to the mass fraction, 40 ~ 50 parts of sec-Butyl Acetates, 3 ~ 6 parts of brassin lactones, 15 ~ 20 parts of steps are taken（3）Spare Rotary evaporation object, 60 ~ 70 parts of dried objects, 4 ~ 7 parts of mixed extracts, 12 ~ 15 parts of hydroxypropyl-β-cyclodextrins, 60 ~ 80 parts of water are mixed It closes, 5 ~ 6h is stirred in 80 ~ 85 DEG C, dry, pulverize 200 mesh sieve, collect sieving particle, obtain rice herbicide.
Embodiment 1
A kind of preparation method of rice herbicide, includes the following steps：
Rice chaff：80 mesh are purchased from Huaiyuan County Wen Bo rice chaff processing factory.Dregs of beans：100 mesh are purchased from Shenzhen Hua Bao feed corporation,Ltds.
Seed activation culture medium：According to the mass fraction, 10 parts of yeast extracts, 15 parts of peptones, 18 parts of glucose are taken, are adjusted Save pH to 6.0,121 DEG C of high pressure sterilization 20min to get.
Mixed extracts：Take Chinese prickly ash, Rhizoma Et Radix Notopterygii in mass ratio 1：2：10 are added the ethanol solution that mass fraction is 80%, through two Carbonoxide supercritical extract, in 40 DEG C, 30MPa, CO2Flow is 15L/h, extracts 1h, obtains mixed extracts.
（1）Take aniline in mass ratio 1：25 are added the aqueous solution of hydrogen bromide that mass fraction is 10%, obtain mixed liquor A, take bromine In mass ratio 1：8 are added the aqueous solution of hydrogen bromide that mass fraction is 10%, obtain mixed liquid B, take mixed liquid B in mass ratio 3：5 are added dropwise To mixed liquor A, time for adding 25min is controlled, 30min is stirred in 20 DEG C, be evaporated under reduced pressure, filtered, taken and filter slag through distillation Water washing obtains washings；
（2）Take washings in mass ratio 1：10 are added glacial acetic acid, are stirred 15min in 20 DEG C, add glacial acetic acid quality 10% Mass fraction be 98% nitric acid, be stirred 20min, obtain stirring mixture, take stirring mixture in mass ratio 10：1：3 add Enter acetic anhydride, glacial acetic acid, keeps the temperature 1h in 25 DEG C, obtain mixture, take mixture in mass ratio 1：100 are added 0 DEG C of distilled water, quiet 2h is set, is evaporated under reduced pressure, takes precipitation；
（3）Take precipitation in mass ratio 2：It is stirred 1h in the sodium bicarbonate solution that 1 addition mass fraction is 5%, filters, takes filter Slag takes aryloxyacetic acid in mass ratio 5：100：2 are added dichloromethane, thionyl chloride, in 75 DEG C of back flow reaction 5h, are evaporated under reduced pressure, It must be evaporated under reduced pressure object a, take filter residue in mass ratio 1：40 are added ethyl acetate, are stirred 20min in 20 DEG C, add filter residue matter The triethylamine of amount 85%, is stirred 5min, obtains mixture a, take mixture a in mass ratio 3：2：10 addition vacuum distillation object a, Ethyl acetate is stirred to react 3h in 2 DEG C, filters, takes filtrate rotary evaporation, obtain rotary evaporation object, spare；
（4）Take dregs of beans in mass ratio 1：3：10 are added rice chaff, deionized water mixing, are stirred 20min in 120rpm, must mix Object adds the alkali protease of mixture quality 1.5%, digests 5h in 55 DEG C, obtains zymolyte, take zymolyte in mass ratio 5：1 The ammonium hydroxide that mass fraction is 10% is added to be stirred, enzyme deactivation filters, takes smoke filtrate to concentrate, obtain concentrate；
（5）It takes candida utili bacterium to be seeded in seed activation culture medium by 2% inoculum concentration, for 24 hours in 25 DEG C of cultures, obtains work Change culture, according to the mass fraction, takes 400 parts of concentrates, 45 parts of activation culture objects, 0.2 part of phytase, 250 parts of water mixing, in 35 DEG C of fermentation 15h, obtain fermentate, dry, obtain dried object；
（6）According to the mass fraction, 40 parts of sec-Butyl Acetates, 3 parts of brassin lactones, 15 parts of steps are taken（3）Spare rotary evaporation Object, 60 parts of dried objects, 4 parts of mixed extracts, 12 parts of hydroxypropyl-β-cyclodextrins, 60 parts of water mixing, 5h is stirred in 80 DEG C, 200 mesh sieve was dry, pulverize, sieving particle is collected, obtains rice herbicide.
Embodiment 2
A kind of preparation method of rice herbicide, includes the following steps：
Rice chaff：80 mesh are purchased from Huaiyuan County Wen Bo rice chaff processing factory.Dregs of beans：100 mesh are purchased from Shenzhen Hua Bao feed corporation,Ltds.
Seed activation culture medium：According to the mass fraction, 15 parts of yeast extracts, 20 parts of peptones, 20 parts of glucose are taken, are adjusted Save pH to 6.0,121 DEG C of high pressure sterilization 20min to get.
Mixed extracts：Take Chinese prickly ash, Rhizoma Et Radix Notopterygii in mass ratio 1：2：10 are added the ethanol solution that mass fraction is 80%, through two Carbonoxide supercritical extract, in 45 DEG C, 30MPa, CO2Flow is 15L/h, extracts 2h, obtains mixed extracts.
（1）Take aniline in mass ratio 1：25 are added the aqueous solution of hydrogen bromide that mass fraction is 10%, obtain mixed liquor A, take bromine In mass ratio 1：8 are added the aqueous solution of hydrogen bromide that mass fraction is 10%, obtain mixed liquid B, take mixed liquid B in mass ratio 3：5 are added dropwise To mixed liquor A, time for adding 30min is controlled, 40min is stirred in 25 DEG C, be evaporated under reduced pressure, filtered, taken and filter slag through distillation Water washing obtains washings；
（2）Take washings in mass ratio 1：10 are added glacial acetic acid, are stirred 20min in 25 DEG C, add glacial acetic acid quality 15% Mass fraction be 98% nitric acid, be stirred 30min, obtain stirring mixture, take stirring mixture in mass ratio 10：1：3 add Enter acetic anhydride, glacial acetic acid, keeps the temperature 2h in 30 DEG C, obtain mixture, take mixture in mass ratio 1：100 are added 2 DEG C of distilled water, quiet 3h is set, is evaporated under reduced pressure, takes precipitation；
（3）Take precipitation in mass ratio 2：It is stirred 2h in the sodium bicarbonate solution that 1 addition mass fraction is 5%, filters, takes filter Slag takes aryloxyacetic acid in mass ratio 5：100：2 are added dichloromethane, thionyl chloride, in 80 DEG C of back flow reaction 6h, are evaporated under reduced pressure, It must be evaporated under reduced pressure object a, take filter residue in mass ratio 1：40 are added ethyl acetate, are stirred 30min in 25 DEG C, add filter residue matter The triethylamine of amount 95%, is stirred 10min, obtains mixture a, take mixture a in mass ratio 3：2：10 addition vacuum distillation object a, Ethyl acetate is stirred to react 4h in 4 DEG C, filters, takes filtrate rotary evaporation, obtain rotary evaporation object, spare；
（4）Take dregs of beans in mass ratio 1：3：10 are added rice chaff, deionized water mixing, are stirred 30min in 120rpm, must mix Object adds the alkali protease of mixture quality 3%, digests 6h in 60 DEG C, obtains zymolyte, take zymolyte in mass ratio 5：1 adds Enter the ammonium hydroxide that mass fraction is 10% to be stirred, enzyme deactivation filters, takes smoke filtrate to concentrate, obtain concentrate；
（5）It takes candida utili bacterium to be seeded in seed activation culture medium by 2% inoculum concentration, cultivates 48h in 30 DEG C, obtain work Change culture, according to the mass fraction, takes 500 parts of concentrates, 50 parts of activation culture objects, 0.4 part of phytase, 300 parts of water mixing, in 45 DEG C of fermentation 20h, obtain fermentate, dry, obtain dried object；
（6）According to the mass fraction, 50 parts of sec-Butyl Acetates, 6 parts of brassin lactones, 20 parts of steps are taken（3）Spare rotary evaporation Object, 70 parts of dried objects, 7 parts of mixed extracts, 15 parts of hydroxypropyl-β-cyclodextrins, 80 parts of water mixing, 6h is stirred in 85 DEG C, 200 mesh sieve was dry, pulverize, sieving particle is collected, obtains rice herbicide.
Embodiment 3
A kind of preparation method of rice herbicide, includes the following steps：
Rice chaff：80 mesh are purchased from Huaiyuan County Wen Bo rice chaff processing factory.Dregs of beans：100 mesh are purchased from Shenzhen Hua Bao feed corporation,Ltds.
Seed activation culture medium：According to the mass fraction, 13 parts of yeast extracts, 17 parts of peptones, 19 parts of glucose are taken, are adjusted Save pH to 6.0,121 DEG C of high pressure sterilization 20min to get.
Mixed extracts：Take Chinese prickly ash, Rhizoma Et Radix Notopterygii in mass ratio 1：2：10 are added the ethanol solution that mass fraction is 80%, through two Carbonoxide supercritical extract, in 43 DEG C, 30MPa, CO2Flow is 15L/h, extracts 1h, obtains mixed extracts.
（1）Take aniline in mass ratio 1：25 are added the aqueous solution of hydrogen bromide that mass fraction is 10%, obtain mixed liquor A, take bromine In mass ratio 1：8 are added the aqueous solution of hydrogen bromide that mass fraction is 10%, obtain mixed liquid B, take mixed liquid B in mass ratio 3：5 are added dropwise To mixed liquor A, time for adding 27min is controlled, 35min is stirred in 23 DEG C, be evaporated under reduced pressure, filtered, taken and filter slag through distillation Water washing obtains washings；
（2）Take washings in mass ratio 1：10 are added glacial acetic acid, are stirred 17min in 23 DEG C, add glacial acetic acid quality 13% Mass fraction be 98% nitric acid, be stirred 25min, obtain stirring mixture, take stirring mixture in mass ratio 10：1：3 add Enter acetic anhydride, glacial acetic acid, keeps the temperature 1h in 27 DEG C, obtain mixture, take mixture in mass ratio 1：100 are added 1 DEG C of distilled water, quiet 2h is set, is evaporated under reduced pressure, takes precipitation；
（3）Take precipitation in mass ratio 2：It is stirred 1h in the sodium bicarbonate solution that 1 addition mass fraction is 5%, filters, takes filter Slag takes aryloxyacetic acid in mass ratio 5：100：2 are added dichloromethane, thionyl chloride, in 77 DEG C of back flow reaction 5h, are evaporated under reduced pressure, It must be evaporated under reduced pressure object a, take filter residue in mass ratio 1：40 are added ethyl acetate, are stirred 25min in 23 DEG C, add filter residue matter The triethylamine of amount 90%, is stirred 7min, obtains mixture a, take mixture a in mass ratio 3：2：10 addition vacuum distillation object a, Ethyl acetate is stirred to react 3h in 3 DEG C, filters, takes filtrate rotary evaporation, obtain rotary evaporation object, spare；
（4）Take dregs of beans in mass ratio 1：3：10 are added rice chaff, deionized water mixing, are stirred 25min in 120rpm, must mix Object adds the alkali protease of mixture quality 2%, digests 5h in 57 DEG C, obtains zymolyte, take zymolyte in mass ratio 5：1 adds Enter the ammonium hydroxide that mass fraction is 10% to be stirred, enzyme deactivation filters, takes smoke filtrate to concentrate, obtain concentrate；
（5）It takes candida utili bacterium to be seeded in seed activation culture medium by 2% inoculum concentration, cultivates 36h in 27 DEG C, obtain work Change culture, according to the mass fraction, takes 450 parts of concentrates, 47 parts of activation culture objects, 0.3 part of phytase, 275 parts of water mixing, in 40 DEG C of fermentation 17h, obtain fermentate, dry, obtain dried object；
（6）According to the mass fraction, 45 parts of sec-Butyl Acetates, 4 parts of brassin lactones, 17 parts of steps are taken（3）Spare rotary evaporation Object, 65 parts of dried objects, 6 parts of mixed extracts, 13 parts of hydroxypropyl-β-cyclodextrins, 70 parts of water mixing, 5h is stirred in 83 DEG C, 200 mesh sieve was dry, pulverize, sieving particle is collected, obtains rice herbicide.
Comparative example：The rice herbicide of company of Zhengzhou City production.
Weedy rices require to carry out according to GB/T 17980.42-2000.Random 3 points of samplings, every 0.25m per cell2, The herbicide of embodiment and comparative example is used to carry out weeding respectively, test result is shown in Table 1.
Table 1：
Test event Embodiment 1 Embodiment 2 Embodiment 3 Comparative example
Green bristlegrass weeding rate % 87 88 86 52~58
Lamb's-quarters weeding rate % 84 83 84 66~71
Amaranth weeding rate % 84 84 85 62~64
Respectively in the latter moon, three months applied for the first time again to carrying out effect experiment for examination weeds, comparison obtains several medicines The drug resistance that object generates is strong and weak.Test result is shown in Table 2.
Table 2：
Test event Embodiment 1 Embodiment 2 Embodiment 3 Comparative example
Control rate % is applied for the first time 86 85 86 66~71
Control rate % is applied after one month 77 75 75 50~53
Cure rate % is applied after three months 71 70 70 32~34
In summary, the herbicide of the invention effect compared with commercial product is more preferable, is worth promoting.

Claims (3)

1. a kind of preparation method of rice herbicide, which is characterized in that the preparation method includes the following steps：
（1）Take aniline in mass ratio 1：25 are added aqueous solution of hydrogen bromide, obtain mixed liquor A, take bromine in mass ratio 1：8 are added bromination Aqueous solution of hydrogen obtains mixed liquid B, takes mixed liquid B in mass ratio 3：5 are added dropwise to mixed liquor A, control 25 ~ 30min of time for adding, in 20 ~ 25 DEG C are stirred, and are evaporated under reduced pressure, and filter, and take and filter slag through distilling water washing, obtain washings；
（2）Take washings in mass ratio 1：10 be added glacial acetic acids, be stirred in 20 ~ 25 DEG C, add glacial acetic acid quality 10 ~ 15% nitric acid, is stirred, and obtains stirring mixture, takes stirring mixture in mass ratio 10：1：3 are added acetic anhydride, glacial acetic acid, In 25 ~ 30 DEG C of heat preservations, mixture is obtained, mixture in mass ratio 1 is taken：100 are added 0 ~ 2 DEG C of distilled water, stand, vacuum distillation, Take precipitation；
（3）Take precipitation in mass ratio 2：It is stirred in 1 addition sodium bicarbonate solution, filters, take filter residue, take aryloxyacetic acid by matter Measure ratio 5：100：2 are added dichloromethane, thionyl chloride, and in 75 ~ 80 DEG C of back flow reactions, vacuum distillation must be evaporated under reduced pressure object a, take Filter residue in mass ratio 1：40 are added ethyl acetate, are stirred in 20 ~ 25 DEG C, add the triethylamine of filter residue quality 85 ~ 95%, It is stirred, obtains mixture a, take mixture a in mass ratio 3：2：10 are added vacuum distillation object a, ethyl acetate, are stirred in 2 ~ 4 DEG C Reaction is mixed, is filtered, is taken filtrate rotary evaporation, obtain rotary evaporation object, it is spare；
（4）Take dregs of beans in mass ratio 1：3：10 are added rice chaff, deionized water mixing, are stirred, obtain mixture, add mixing The alkali protease of amount of substance 1.5 ~ 3% obtains zymolyte, takes zymolyte in mass ratio 5 in 55 ~ 60 DEG C of enzymolysis：1 addition ammonium hydroxide stirs Mixing is mixed, enzyme deactivation filters, takes smoke filtrate to concentrate, obtain concentrate；
（5）It takes candida utili bacterium to be seeded in seed activation culture medium by 2% inoculum concentration, in 25 ~ 30 DEG C of cultures, obtains work Change culture and takes 400 ~ 500 parts of concentrates, 45 ~ 50 parts of activation culture objects, 0.2 ~ 0.4 part of phytase, 250 according to the mass fraction ~ 300 parts of water mixing obtain fermentate in 35 ~ 45 DEG C of fermentations, dry, obtain dried object；
（6）According to the mass fraction, 40 ~ 50 parts of sec-Butyl Acetates, 3 ~ 6 parts of brassin lactones, 15 ~ 20 parts of steps are taken（3）Spare Rotary evaporation object, 60 ~ 70 parts of dried objects, 4 ~ 7 parts of mixed extracts, 12 ~ 15 parts of hydroxypropyl-β-cyclodextrins, 60 ~ 80 parts of water are mixed It closes, is stirred in 80 ~ 85 DEG C, dry, pulverize sieving, collect sieving particle, obtain rice herbicide.
2. the preparation method of rice herbicide according to claim 1, which is characterized in that the step（5）Middle seed is lived Change culture medium：According to the mass fraction, 10 ~ 15 parts of yeast extracts, 15 ~ 20 parts of peptones, 18 ~ 20 parts of glucose are taken, pH is adjusted To 6.0,121 DEG C of high pressure sterilization 20min to get.
3. the preparation method of rice herbicide according to claim 1, which is characterized in that the step（6）Middle mixing extraction Take object：Take Chinese prickly ash, Rhizoma Et Radix Notopterygii in mass ratio 1：2：10 are added ethanol solutions, through carbon dioxide supercritical extraction, in 40 ~ 45 DEG C, 30MPa、CO2Flow is 15L/h, extracts 1 ~ 2h, obtains mixed extracts.
CN201810463129.4A 2018-05-15 2018-05-15 A kind of preparation method of rice herbicide Pending CN108522564A (en)

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JPS4837819B1 (en) * 1965-05-11 1973-11-14
CN101919494A (en) * 2010-09-30 2010-12-22 大连三科生物工程有限公司 Complex microorganism additive as well as preparation method and application thereof
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CN105941485A (en) * 2016-05-14 2016-09-21 尤馨雅 Efficient garden herbicide
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Application publication date: 20180914