CN107296044B - Plant-source pesticide surfactant and preparation method and application thereof - Google Patents

Plant-source pesticide surfactant and preparation method and application thereof Download PDF

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CN107296044B
CN107296044B CN201710562488.0A CN201710562488A CN107296044B CN 107296044 B CN107296044 B CN 107296044B CN 201710562488 A CN201710562488 A CN 201710562488A CN 107296044 B CN107296044 B CN 107296044B
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surfactant
pesticide
dregs
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sophora alopecuroide
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CN107296044A (en
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魏凤彪
朱建伟
徐向荣
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Beijing Kingbo Biotech Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, 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
    • A01N25/30Biocides, 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
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
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  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to the field of pesticides, and particularly discloses a botanical pesticide surfactant and a preparation method thereof. The botanical pesticide surfactant is prepared by soaking bitter bean dregs in water, grinding to obtain bitter bean dreg slurry, carrying out enzymolysis reaction by pepsin, papain or bromelain, and separating insoluble substances. The plant source pesticide surfactant is a biological compound with surface activity extracted from plants, has the advantages of no toxicity, biodegradability and the like besides the physicochemical characteristics of a chemical synthetic surfactant, has a very wide application prospect, and can possibly become a substitute or an upgraded substitute of the chemical synthetic surfactant.

Description

Plant-source pesticide surfactant and preparation method and application thereof
Technical Field
The invention relates to the field of pesticides, and particularly relates to a botanical pesticide surfactant.
Background
The surfactant in the pesticide is one of indispensable components for preparing pesticide raw materials which cannot be directly used into usable pesticide preparations. The pesticide adjuvant is applied to pesticides, can improve the using effect of the pesticides, can reduce the using amount of the pesticides, reduces the influence of the pesticides on the environment, and brings great benefit to agricultural production. However, since the pesticide is a special chemical with very strong biological activity, the object prevention and control, object protection and environmental conditions are very complicated, and the surfactant in the pesticide needs to be selected and prepared according to the properties and characteristics of the original pesticide, and the influence of the surfactant on the target organism needs to be considered.
The main applications of the current pesticide surfactants are: fatty alcohol polyoxyethylenes, alkylphenol ethoxylates, sulfonates, amides, silicones, and the like, but are all made by petrochemical cracking or chemical synthesis.
The research on the surface activity of Chinese pesticide preparations starts from the 50 th of the 20 th century and starts to produce in batches in the 60 th of the 20 th century, and the main products are: the emulsifier comprises anionic, nonionic and nonionic compounded surfactant. Agricultural emulsifier monomers such as calcium dodecylbenzenesulfonate (agricultural emulsifier 500), nonylphenol polyoxyethylene ether (agricultural emulsifier 100), dibenzylphenol polyoxyethylene ether (agricultural emulsifier 300), benzyl dimethylphenol polyoxyethylene ether (agricultural emulsifier 400), phenethylphenol polyoxyethylene ether (agricultural emulsifier 600), alkylphenol formaldehyde resin polyoxyethylene ether (agricultural emulsifier 700), phenethylphenol polyoxyethylene polyoxypropylene ether (agricultural emulsifier 1600) and the like. The compounded pesticide emulsifier such as 0201, 0203B, 0204C and the like can basically meet the requirements of missible oil preparations.
However, with the development of science and technology and the growing concern on food safety, most of the solvents in the original traditional surfactants are organic solvents such as toluene, xylene and methanol, and the solvents pose more or less threat and pollution to human health and environment when in use. A large class of alkylphenol polyoxyethylene ether in the traditional agricultural surfactant is forbidden to be used in the national standard GB/T13171-2004 of Chinese washing powder. They are highly toxic to fish and are also difficult to biodegrade, and in addition, impurities entrained during their production have carcinogenic activity.
In addition, in recent years, with the withdrawal of some highly toxic chemical pesticides from the market, development of an environmentally friendly plant-derived pesticide is indispensable, but it is difficult to fully exert the characteristics of a plant-derived pesticide with a conventional surfactant.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide an agricultural surfactant which is environment-friendly and is derived from plants, reduce the harm of harmful solvents in the traditional surfactant and solve the problem that no proper surfactant exists in the plant-derived pesticide at present.
The surfactant as an adjuvant for agricultural chemicals should have the following basic properties: the pesticide is suitable for the purpose of processing and applying pesticides, and is beneficial to full play of pesticide effect; secondly, the pesticide is safe to crops under actual use conditions and has low toxicity to people, livestock and fishes; secondly, the prepared agent is stable, does not deteriorate in the effective storage period, and is convenient and safe to use; finally, the resource is rich and the cost is low.
In order to realize the purpose of the invention, the technical scheme of the invention is as follows:
in a first aspect, the invention provides a plant-derived pesticide surfactant, and a preparation method thereof comprises the following steps:
(1) soaking the bitter bean dregs in water, and grinding to obtain a bitter bean dreg slurry A;
(2) dissolving pepsin, papain or bromelain in warm water to obtain a protease solution B;
(3) adjusting the pH value of the fenugreek dreg slurry A to 2, adding a protease solution B, and carrying out enzymolysis reaction; after the enzymolysis is finished, carrying out inactivation treatment on the enzyme, and adjusting the pH value of an enzymolysis solution to 6.5;
(4) and separating insoluble substances of the enzymolysis solution to obtain a solution C, namely the botanical pesticide surfactant.
Furthermore, the sophora alopecuroide dregs are the sophora alopecuroide dregs left after the sophora alopecuroide is extracted by 70 percent ethanol and matrine is carried out.
Preferably, the temperature of the enzymolysis reaction in the step (3) is 55-65 ℃, and the reaction is carried out for 8-12 hours.
Preferably, the weight of the pepsin, papain or bromelain is 0.5-2% of the weight of the sophora alopecuroide pulp A.
Preferably, the fenugreek dregs are added into water to be soaked for 24 hours at 45 ℃ and ground for 3 hours to obtain the fenugreek dreg slurry A.
Preferably, the mass ratio of the bitter bean dregs to the water is 1: 5.
Further, pepsin, papain or bromelain was dissolved in warm water at 30 ℃ to obtain a protease solution B.
Further, the inactivation treatment of the enzyme is specifically as follows: the temperature was raised to 80 ℃ for 30 minutes.
In a second aspect, the invention provides a preparation method of a plant-derived pesticide surfactant, which comprises the following steps:
(1) adding the bitter bean dregs into water, soaking for 24 hours at 45 ℃, and grinding for 3 hours to obtain bitter bean dreg slurry A; wherein the mass ratio of the fenugreek dregs to the water is 1: 5;
(2) dissolving pepsin, papain or bromelain in warm water at 30 ℃ to obtain a protease solution B;
(3) adding the fenugreek dreg slurry A into a heating reaction kettle, adjusting the pH to 2 by using dilute hydrochloric acid, adding a protease solution B, heating to 60 ℃, stirring once every half hour, and continuously reacting for 12 hours; then, heating the reaction kettle to 80 ℃ and keeping the temperature for 30 minutes to inactivate the protease; adding sodium hydroxide solution into the reaction kettle to adjust the pH value to 6.5;
wherein, the weight of the protease in the protease solution B is one percent of the weight of the fenugreek dreg slurry A;
(4) and (3) taking the liquid in the reaction kettle, and separating out insoluble substances by using a centrifugal machine to obtain the plant source pesticide surfactant.
In a third aspect, the invention provides an application of the plant-derived pesticide surfactant in preparation of pesticides.
Preferably, the active ingredient of the pesticide is derived from natural plants and is not chemically synthesized.
The raw materials or reagents involved in the invention are all common commercial products, and the operations involved are all routine operations in the field unless otherwise specified.
The above-described preferred conditions may be combined with each other to obtain a specific embodiment, in accordance with common knowledge in the art.
The invention has the beneficial effects that:
the invention provides a plant source surfactant, which is a biological compound with surface activity extracted from plants, has the advantages of no toxicity, biodegradability and the like besides the physicochemical characteristics of a chemical synthetic surfactant, has very wide application prospect, and can possibly become a substitute or an upgraded substitute of the chemical synthetic surfactant.
Detailed Description
Preferred embodiments of the present invention will be described in detail with reference to the following examples. It is to be understood that the following examples are given for illustrative purposes only and are not intended to limit the scope of the present invention. Various modifications and alterations of this invention will become apparent to those skilled in the art without departing from the spirit and scope of this invention.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1 botanical pesticide surfactant
This example illustrates a plant-derived pesticidal surfactant and a method for preparing the same according to the present invention.
The raw material is the sophora alopecuroide dregs which are obtained by the inner Mongolia Qingyuan biological science and technology limited company after the sophora alopecuroide is extracted by ethanol to obtain the sophora alopecuroide dregs.
The preparation method of the plant source pesticide surfactant is preferably as follows:
(1) adding the bitter bean dregs into water, soaking for 24 hours at 45 ℃, and grinding for 3 hours to obtain bitter bean dreg slurry A; wherein the mass ratio of the fenugreek dregs to the water is 1: 5;
(2) dissolving pepsin, papain or bromelain in warm water at 30 ℃ to obtain a protease solution B;
(3) adding the fenugreek dreg slurry A into a heating reaction kettle, adjusting the pH to 2 by using dilute hydrochloric acid, adding a protease solution B, heating to 60 ℃, stirring once every half hour, and continuously reacting for 12 hours; then, heating the reaction kettle to 80 ℃ and keeping the temperature for 30 minutes to inactivate the protease; adding sodium hydroxide solution into the reaction kettle to adjust the pH value to 6.5;
wherein, the weight of the protease in the protease solution B is one percent of the weight of the fenugreek dreg slurry A;
(4) and (3) taking the liquid in the reaction kettle, and separating out insoluble substances by using a centrifugal machine to obtain the plant source pesticide surfactant.
Example 2 emulsifying Properties of botanical pesticide surfactants
Firstly, experimental raw materials and instruments:
1. experiment raw materials: peanut oil
2. The instrument comprises the following steps: centrifuge (Xiang instrument TDZ5-WS), beaker and graduated cylinder
II, an experimental method:
measurement of emulsion stability
Adding 1% of the plant source pesticide surfactant obtained in example 1 into oil and water in a ratio of 1:9, uniformly stirring and mixing to prepare an emulsion, transferring the emulsion into a graduated centrifuge tube, centrifuging at 4000rpm for 15min, reading the volume of an emulsified phase, and calculating the result according to the following formula:
emulsion stability% (% emulsion layer height/total liquid height × 100%
The values obtained are: 76.3 percent.
The plant source pesticide surfactant provided by the invention is proved to have stronger emulsifying capacity and stability.
Example 3 field test of plant-derived surfactants
First, demonstration purpose
Through experiments, the control effect of the plant source surfactant and the traditional agricultural surfactant agricultural emulsion 500# on vegetable aphids in the field is tested by taking 7.5% rotenone emulsifiable concentrate as an example.
Second, demonstration of the drug
1. Exemplary agents: 7.5% rotenone emulsifiable concentrate A;
taking 100 g of 7.5 percent rotenone emulsifiable solution A as an example, the preparation method comprises the following steps:
(1) accurately weighing 7.5 g of rotenone, and putting the rotenone into a 200mL beaker;
(2) adding 30 g of cyclohexanone into a weighed rotenone beaker, and fully stirring for 15 minutes to completely dissolve solid substances;
(3) adding 15 g of the plant source pesticide surfactant obtained in the example 1 into the dissolved cyclohexanone solution, and stirring for 15 minutes;
(4) 47.5 g of xylene was further added and stirred for 30 minutes to obtain 7.5% rotenone cream A.
2. Control agents: 7.5% rotenone emulsifiable concentrate B; the difference between the pesticide emulsion and 7.5% rotenone emulsifiable solution A is that the plant source surfactant is replaced by agricultural emulsion 500 #.
The preparation method comprises the following steps:
(1) accurately weighing 7.5 g of rotenone, and putting the rotenone into a 200mL beaker;
(2) adding 30 g of cyclohexanone into a weighed rotenone beaker, and fully stirring for 15 minutes to completely dissolve solid substances;
(3) adding 15 g of agricultural milk 500# into the dissolved cyclohexanone solution, and stirring for 15 minutes;
(4) 47.5 g of xylene was further added and stirred for 30 minutes to obtain 7.5% rotenone cream A.
Third, demonstration crops and control objects
1. Demonstration crops: chinese cabbage, variety: and (4) enabling people to live in summer.
2. The control object is: aphids.
Fourth, demonstration design
Treatment of Demonstration medicament Treatment dosage (g or ml/mu) Demonstration area
1 7.5% Rotenone emulsifiable concentrate A 50 2.5hm2
2 7.5% Rotenone emulsifiable concentrate B 50 2.5hm2
3(CK) Clean water / 20m2
The exemplary large area contrast method is used without repetition.
Fifth, exemplary basic situation
Demonstrating that the experimental soil is loam, the pH value is 6.8, the organic matter content is 2.6 percent and the fertility is general in a Handan Yongnian county vegetable planting base in Hebei province. During the test, the Chinese cabbage is in 11-13 leaf stage, and no pesticide is used 20 days before the test. The medicine is applied 16 days after 8 months and 10 days, wherein the application day is cloudy and the medicine is blown to 1-grade northern wind. During the test period, no rainfall occurs, and the daily average temperature is 27.3-30.8 ℃.
Sixthly, pesticide application and control effect investigation
1. Application of the medicine: at 16 days 10.8 months, applying conventional spray at initial stage of aphid initiation, and manually spraying with HD-400 of Singapore LinongThe liquid consumption of the sprayer is 900kg/hm2
2. During the test period: the weather condition is good, no rain and breeze.
3. The investigation method comprises the following steps: the tests respectively take samples at 5 points in each cell before and 1 day, 3 days, 7 days and 14 days after the pesticide, each point has 5 plants, each plant has 2 insect leaves, the number of the living aphids is investigated and recorded, the control effect is corrected, the test also investigates the influence of pesticide application on the growth, leaf color and the like of the Chinese cabbage after the pesticide application, and the safety is investigated.
4. Drug effect calculation method
Figure BDA0001347502500000071
Figure BDA0001347502500000072
Seven, fruit and analysis
And (3) safety analysis: after the application, no adverse effect on the growth of the Chinese cabbage is found in each medicament treatment area, which shows that the two 7.5% rotenone emulsifiable concentrates are safe and harmless to the Chinese cabbage under the demonstration dosage.
1. The prevention and treatment effect is as follows: see table 1.
TABLE 17.5% Rotenone emulsifiable concentrate aphid prevention and control field popularization test result statistical table
Figure BDA0001347502500000073
Figure BDA0001347502500000081
According to the statistical table of the field popularization test results of preventing and controlling aphids by 7.5% rotenone missible oil, under the condition of using the same dosage, the control effects of 7.5% rotenone missible oil A and B in one day are respectively 43.0% and 42.9%, and the control effects in three days after the pesticide are respectively 67.5% and 65.0%. The control effect of the traditional Chinese medicine composition is 83.1 percent and 78.5 percent respectively in seven days after the application, and the control effect of the traditional Chinese medicine composition is 80.8 percent and 76.0 percent respectively in fourteen days after the application.
Eight, evaluation and suggestion
7.5 Rotenone emulsifiable concentrate A (prepared from plant source surfactant) has better field test effect than 7.5 Rotenone emulsifiable concentrate B (prepared from Nongru 500 #).
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (4)

1. A plant source pesticide surfactant is characterized in that the preparation method comprises the following steps:
(1) adding the bitter bean dregs into water, soaking for 24 hours at 45 ℃, and grinding for 3 hours to obtain bitter bean dreg slurry A, wherein the mass ratio of the bitter bean dregs to the water is 1: 5; the sophora alopecuroide dregs are the sophora alopecuroide dregs left after the sophora alopecuroide is extracted by 70 percent ethanol and matrine is carried out;
(2) dissolving pepsin, papain or bromelain in warm water at 30 ℃ to obtain a protease solution B; the weight of the pepsin, the papain or the bromelain is 1 percent of that of the sophora alopecuroide dreg serous fluid A;
(3) adjusting the pH value of the sophora alopecuroide dreg slurry A to 2, adding a protease solution B, and carrying out an enzymolysis reaction at the temperature of 60 ℃ while stirring once every half hour for 12 hours; after the enzymolysis is finished, carrying out inactivation treatment on the enzyme, and adjusting the pH value of an enzymolysis solution to 6.5; carrying out inactivation treatment on the enzyme, namely heating to 80 ℃ and keeping for 30 minutes;
(4) and separating insoluble substances of the enzymolysis solution to obtain a solution C, namely the botanical pesticide surfactant.
2. A preparation method of a plant source pesticide surfactant is characterized by comprising the following steps:
(1) adding the bitter bean dregs into water, soaking for 24 hours at 45 ℃, and grinding for 3 hours to obtain bitter bean dreg slurry A; wherein the mass ratio of the fenugreek dregs to the water is 1: 5; the sophora alopecuroide dregs are the sophora alopecuroide dregs left after the sophora alopecuroide is extracted by 70 percent ethanol and matrine is carried out;
(2) dissolving pepsin, papain or bromelain with the mass fraction of the fenugreek dreg slurry A being 1% in warm water at the temperature of 30 ℃ to obtain a protease solution B;
(3) adding the fenugreek dreg slurry A into a heating reaction kettle, adjusting the pH to 2 by using dilute hydrochloric acid, adding a protease solution B, heating to 60 ℃, stirring once every half hour, and continuously reacting for 12 hours; then, heating the reaction kettle to 80 ℃ and keeping the temperature for 30 minutes to inactivate the protease; adding sodium hydroxide solution into the reaction kettle to adjust the pH value to 6.5;
(4) and (3) taking the liquid in the reaction kettle, and separating out insoluble substances by using a centrifugal machine to obtain the plant source pesticide surfactant.
3. The use of the plant-derived pesticidal surfactant of claim 1 in the preparation of a pesticide.
4. Use according to claim 3, characterized in that the active ingredient of the pesticide is derived from plants.
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