CN106929031A - It is a kind of with broad spectrum disinfestation and the good Nutrition Soil of water retention property and preparation method thereof - Google Patents
It is a kind of with broad spectrum disinfestation and the good Nutrition Soil of water retention property and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, 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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- 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
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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
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/24—Lauraceae [Laurel family], e.g. laurel, avocado, sassafras, cinnamon or camphor
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- C07D471/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
- C07D471/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed systems contains four or more hetero rings
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
It is a kind of with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that extracted and separating matrine using ultrasonic extraction and Microwave Extraction GC-MS and chloroform extraction first；Again by attapulgite, vermiculite, zeolite heating using microwave, increased its effective aperture, matrine is entered in its aperture by ultrasonic vibration；It is last under the catalysis of potassium peroxydisulfate, with attapulgite, vermiculite, zeolite cross-linked polymeric, to form the inorganic ore polymer beads of spatial networks with acrylamide as monomer, obtain with broad spectrum disinfestation and the good Nutrition Soil of water retention property.It is of the invention with broad spectrum disinfestation, soil texture, the lifting soil organism to be improved with broad spectrum disinfestation and the good Nutrition Soil of water retention property, adjust Soil Micro-environment, it is adaptable to plant flowers and nursery stock.
Description
Technical field
The invention belongs to agriculture field, and in particular to it is a kind of with broad spectrum disinfestation and the good Nutrition Soil of water retention property and its
Preparation method.
Background technology
In agricultural pollution source, pollution by pesticides is the one side of most serious.It is a large amount of to use severe toxicity, the broad spectrum activity of high residue
Chemical pesticide, not only causes farmland and agricultural product Pesticides content severe overweight, but also often results in people, animal poisoning,
Threaten the life and health of people.In order to fundamentally change this situation, it is necessary to use efficient, low toxicity or nontoxic, low residual
Stay or noresidue botanical pesticide.Numerous species in plant contain the composition for killing pest and disease damage, after entering industrialization extraction,
Can be used as agricultural chemicals, i.e. botanical pesticide.Most plant pesticide low toxicities, do not destroy ecological environment, and residual is few, selectivity
By force, pest natural enemy, insect and germ are not killed plant pesticide is difficult to develop immunity to drugs, serviceable bife is long, and consumption is few, uses
Low cost.Using plant pesticide, for promoting agricultural sustainable development, with extremely important realistic meaning.Kuh-seng is pulse family
Plant kuh-seng（Sophora flavescens Ait）Root, have heat-clearing and damp-drying drug, desinsection, the effects such as diuresis.Kuh-seng is in medicine, beast
The aspects such as medicine, agricultural chemicals, environmental sanitation medication are of wide application, and are a kind of rising botanical pesticide resources.
Tian Benzhi et al. exists《Prevention effect of the kuh-seng aqueous emulsion of biological pesticide 2% to cabbage caterpillar》Experimental study table in one text
Bright, 2% kuh-seng aqueous emulsion is a kind of good medicament for preventing and treating brassicaceous vegetable (Chinese cabbage) insect cabbage caterpillar.The medicament has
Have good disinsection effect, do not injure natural enemy, it is free from environmental pollution the features such as, safety is grown to Chinese cabbage, and the lasting period is also more long.
The content of the invention
It is an object of the invention to provide a kind of with broad spectrum disinfestation and the good Nutrition Soil of water retention property and its preparation side
Method.
To achieve these goals, present invention employs following technical scheme：
It is a kind of with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that first using ultrasonic extraction and microwave
GC-MS and chloroform extraction is extracted to extract and separating matrine；Again by attapulgite, vermiculite, zeolite heating using microwave,
Increased its effective aperture, matrine is entered in its aperture by ultrasonic vibration；Finally with acrylamide as monomer,
Under the catalysis of potassium peroxydisulfate, with attapulgite, vermiculite, zeolite cross-linked polymeric, the inorganic ore-polymer particles of spatial networks are formed
Grain, obtains with broad spectrum disinfestation and the good Nutrition Soil of water retention property.
It is described with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that it is by following weight portion
Raw material is prepared from：Kuh-seng 25-30 parts, 6-8 parts of anise, Gui Ye 5-6 parts, attapulgite 50-60 parts, vermiculite 20-30 parts, zeolite
20-30 parts, sodium pyrophosphate 6-8 parts, acrylyl oxy-ethyl-trimethyl salmiac 12-15 parts, persulfate aqueous solution 20-25 parts,
Copper sulphate 5-6 parts, magnesium sulfate 6-8 parts, ammonium molybdate 3-4 parts, potassium chloride 10-12 parts, acrylamide 30-35 parts, the second of 70-75%
Appropriate alcohol solution, appropriate aqueous hydrochloric acid solution, appropriate chloroform, appropriate deionized water.
It is described with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that it is by steps system
It is standby to form：
（1）Kuh-seng, anise, Gui Ye are cleaned 2-3 times with deionized water, natural air drying；Attrition grinding 50-60min, crosses 80-100
Mesh sieve, obtains granulate mixture；Granulate mixture using 70-75% ethanol water ultrasonic extraction 2-3 times, each ultrasound is carried
The condition for taking is：Solid-liquid ratio is 7-8, and ultrasonic extraction temperature is 50-60 DEG C, and ultrasonic power is 300-400W, during ultrasonic extraction
Between 30-40min；Filtering, collects filtrate, and filtrate is reclaimed ethanol by merging filtrate by 65-70 DEG C of vacuum distillation, and distillation is treated
With；
（2）Filter cake is used into aqueous hydrochloric acid solution microwave abstracting 3-4 times, the condition of each microwave abstracting is：PH is 3-4, solid-liquid ratio
It is 10-11, microwave power is 500-550w, and radiated time is 20-25min, filtering collects filtrate, by filtrate and step（1）'s
Distillation merges, and is concentrated under reduced pressure into liquid volume and reduces 2/3；Regulation PH is 10-11, using chloroform extraction 2-3 times, every time
The condition of extraction is：Water phase is 3-4 with the volume ratio of organic phase：1, merge organic phase, reclaim three by 50-60 DEG C of vacuum distillation
Chloromethanes, obtains matrine crude oil；
（3）By attapulgite, vermiculite, zeolite co-grinding grinding 50-60min, 200-250 mesh sieves are crossed, obtain hybrid particles；Will
Hybrid particles are transferred in micro-wave oven, and with the heats 15-20min of 500-600W, cooling is taken out standby；
（4）By step（2）Product, step（3）Product and sodium pyrophosphate be added to equivalent to step（3）Products weight part
In 10-12 times of deionized water, ultrasonic vibration 40-50min；Acrylyl oxy-ethyl-trimethyl salmiac is added, is mixed equal
After even, 45-50 DEG C is warming up to, leads to nitrogen 30-40min, add 1/5 persulfate aqueous solution, magnetic agitation reacts 4-5h, cold
But to room temperature；Copper sulphate, magnesium sulfate, ammonium molybdate, potassium chloride, acrylamide are added, 45-50 DEG C is warming up to, magnetic agitation makes
It is completely dissolved, and keeps system temperature constant, leads to nitrogen 30-40min, at the uniform velocity adds 3/5 potassium peroxydisulfate in 8-10h thereafter
The aqueous solution, reacts 8-10h, disposably adds remaining persulfate aqueous solution, continues magnetic agitation reaction 4-5h, filtering, water
Wash, dry, obtain a kind of with broad spectrum disinfestation and the good Nutrition Soil of water retention property.
It is described with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that described aqueous hydrochloric acid solution
Concentration be 2-3mol/L.
It is described with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that described potassium peroxydisulfate water
The concentration of solution is 0.3-0.4mol/L.
Using above-mentioned technical scheme, beneficial effects of the present invention are：
The present invention first crushes kuh-seng, then using ultrasonator ultrasonic extraction, using the cavitation effect of ultrasound, fuel factor and machine
Tool effect is acted on, and when the ul-trasonic irradiation of big energy is in kuh-seng, kuh-seng cell membrane and organism is existed under larger pressure
Moment ruptures, and substantially reduces the extraction time of matrine, and the effect of vibration of ultrasonic wave strengthens the release of intracellular matrine,
So as to improve the recovery rate of matrine.The filter cake that the present invention will be obtained after ultrasonic extraction again has by microwave abstracting, microwave
Penetrability, makes polar molecule and group produce heat with microwave high-frequency concussion, can be simultaneously rapid in reactant internal and external parts, equal
Heat evenly；Remaining matrine in filter cake is extracted, the recovery rate of matrine is further increased.The present invention is additionally added
Anistree and osmanthus leaf, aniseed essential oil and osmanthus leaf essential oil have antifeedant activity, further increase the insecticidal activity of matrine to insect.
Attapulgite, vermiculite, zeolite heating using microwave are increased its effective aperture by the present invention, and matrine is made by ultrasonic vibration
Into in its aperture, not only the gentle On The Drug Release of fertilizer conservation, water conservation, and matrine can be played a part of with improved soil structure
Slow release, extends matrine action time, and can significantly reduce its resolution ratio in storage.The present invention is with acryloyl
Amine is monomer, under the catalysis of potassium peroxydisulfate, with attapulgite, vermiculite, zeolite cross-linked polymeric, forms the inorganic ore deposit of spatial networks
Stone-polymer beads, the effect of the gentle On The Drug Release of further have additional nutrients native fertilizer conservation, water conservation.It is of the invention with broad spectrum disinfestation
Property and the good Nutrition Soil of water retention property, with broad spectrum disinfestation, can improve soil texture, lifting the soil organism, regulation soil
Earth microenvironment, it is adaptable to plant flowers and nursery stock.
Specific embodiment
The present embodiment with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is prepared by the raw material of following weight portion
Form：25 parts of kuh-seng, anistree 8 parts, 6 parts of Gui Ye, 60 parts of attapulgite, 30 parts of vermiculite, 30 parts of zeolite, 8 parts of sodium pyrophosphate, propylene
15 parts of acyloxyethyl trimethyl ammonium chloride, 25 parts of persulfate aqueous solution, 6 parts of copper sulphate, 8 parts of magnesium sulfate, 4 parts of ammonium molybdate, chlorine
Change 12 parts of potassium, 35 parts of acrylamide, appropriate 75% ethanol water, appropriate aqueous hydrochloric acid solution, appropriate chloroform, deionization
Appropriate amount of water.
The present embodiment with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is prepared from by the steps：
（1）Kuh-seng, anise, Gui Ye are cleaned into 3 times, natural air drying with deionized water；Attrition grinding 60min, crosses 100 mesh sieves, obtains
To granulate mixture；Granulate mixture using 75% ethanol water ultrasonic extraction 2-3 times, the condition of each ultrasonic extraction is：
Solid-liquid ratio is 7, and ultrasonic extraction temperature is 60 DEG C, and ultrasonic power is 400W, ultrasonic extraction time 30min；Filtering, collects filter
Filtrate is reclaimed ethanol by liquid, merging filtrate by 70 DEG C of vacuum distillations, and distillation is stand-by；
（2）Filter cake is used into aqueous hydrochloric acid solution microwave abstracting 4 times, the condition of each microwave abstracting is：PH is 3, and solid-liquid ratio is 10,
Microwave power is 550w, and radiated time is 25min, filtering, filtrate is collected, by filtrate and step（1）Distillation merge, decompression
It is concentrated into liquid volume and reduces 2/3；Regulation PH is 11, and using chloroform extraction 3 times, the condition of extraction is every time：Water phase with
The volume ratio of organic phase is 4：1, merge organic phase, chloroform is reclaimed by 60 DEG C of vacuum distillations, obtain matrine crude oil；
（3）By attapulgite, vermiculite, zeolite co-grinding grinding 60min, 250 mesh sieves are crossed, obtain hybrid particles；Will mixing
Grain is transferred in micro-wave oven, and with the heats 15min of 600W, cooling is taken out standby；
（4）By step（2）Product, step（3）Product and sodium pyrophosphate be added to equivalent to step（3）Products weight part
In 12 times of deionized water, ultrasonic vibration 50min；Acrylyl oxy-ethyl-trimethyl salmiac is added, after mixing and stirring, is risen
Temperature leads to nitrogen 40min to 50 DEG C, adds 1/5 persulfate aqueous solution, magnetic agitation reaction 5h to be cooled to room temperature；Add
Copper sulphate, magnesium sulfate, ammonium molybdate, potassium chloride, acrylamide, are warming up to 50 DEG C, and magnetic agitation is completely dissolved it, keep system
Temperature is constant, leads to nitrogen 40min, at the uniform velocity adds 3/5 persulfate aqueous solution in 10h thereafter, reacts 10h, disposable to add
Enter remaining persulfate aqueous solution, continue magnetic agitation and react 5h, filtering, washing is dried, and obtains a kind of with broad spectrum disinfestation
Property and the good Nutrition Soil of water retention property.
The concentration of the aqueous hydrochloric acid solution of the present embodiment is 3mol/L.
The concentration of the persulfate aqueous solution of the present embodiment is 0.4mol/L.
Claims (5)
1. a kind of with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that first using ultrasonic extraction with it is micro-
Ripple extracts GC-MS and chloroform extraction to extract and separating matrine；Attapulgite, vermiculite, zeolite microwave are added again
Heat, is increased its effective aperture, matrine is entered in its aperture by ultrasonic vibration；It is finally single with acrylamide
Body, under the catalysis of potassium peroxydisulfate, and attapulgite, vermiculite, zeolite cross-linked polymeric form the inorganic ore of spatial networks-poly-
Polymer beads, obtain with broad spectrum disinfestation and the good Nutrition Soil of water retention property.
2. according to claims 1 with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that its by
The raw material of following weight portion is prepared from：Kuh-seng 25-30 parts, 6-8 parts of anise, Gui Ye 5-6 parts, attapulgite 50-60 parts, vermiculite
20-30 parts, zeolite 20-30 parts, sodium pyrophosphate 6-8 parts, acrylyl oxy-ethyl-trimethyl salmiac 12-15 parts, potassium peroxydisulfate water
Solution 20-25 parts, copper sulphate 5-6 parts, magnesium sulfate 6-8 parts, ammonium molybdate 3-4 parts, potassium chloride 10-12 parts, acrylamide 30-35
Part, the appropriate ethanol water of 70-75%, appropriate aqueous hydrochloric acid solution, appropriate chloroform, appropriate deionized water.
3. according to claims 1 with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that its by
The steps is prepared from：
（1）Kuh-seng, anise, Gui Ye are cleaned 2-3 times with deionized water, natural air drying；Attrition grinding 50-60min, crosses 80-100
Mesh sieve, obtains granulate mixture；Granulate mixture using 70-75% ethanol water ultrasonic extraction 2-3 times, each ultrasound is carried
The condition for taking is：Solid-liquid ratio is 7-8, and ultrasonic extraction temperature is 50-60 DEG C, and ultrasonic power is 300-400W, during ultrasonic extraction
Between 30-40min；Filtering, collects filtrate, and filtrate is reclaimed ethanol by merging filtrate by 65-70 DEG C of vacuum distillation, and distillation is treated
With；
（2）Filter cake is used into aqueous hydrochloric acid solution microwave abstracting 3-4 times, the condition of each microwave abstracting is：PH is 3-4, solid-liquid ratio
It is 10-11, microwave power is 500-550w, and radiated time is 20-25min, filtering collects filtrate, by filtrate and step（1）'s
Distillation merges, and is concentrated under reduced pressure into liquid volume and reduces 2/3；Regulation PH is 10-11, using chloroform extraction 2-3 times, every time
The condition of extraction is：Water phase is 3-4 with the volume ratio of organic phase：1, merge organic phase, reclaim three by 50-60 DEG C of vacuum distillation
Chloromethanes, obtains matrine crude oil；
（3）By attapulgite, vermiculite, zeolite co-grinding grinding 50-60min, 200-250 mesh sieves are crossed, obtain hybrid particles；Will
Hybrid particles are transferred in micro-wave oven, and with the heats 15-20min of 500-600W, cooling is taken out standby；
（4）By step（2）Product, step（3）Product and sodium pyrophosphate be added to equivalent to step（3）Products weight part
In 10-12 times of deionized water, ultrasonic vibration 40-50min；Acrylyl oxy-ethyl-trimethyl salmiac is added, is mixed equal
After even, 45-50 DEG C is warming up to, leads to nitrogen 30-40min, add 1/5 persulfate aqueous solution, magnetic agitation reacts 4-5h, cold
But to room temperature；Copper sulphate, magnesium sulfate, ammonium molybdate, potassium chloride, acrylamide are added, 45-50 DEG C is warming up to, magnetic agitation makes
It is completely dissolved, and keeps system temperature constant, leads to nitrogen 30-40min, at the uniform velocity adds 3/5 potassium peroxydisulfate in 8-10h thereafter
The aqueous solution, reacts 8-10h, disposably adds remaining persulfate aqueous solution, continues magnetic agitation reaction 4-5h, filtering, water
Wash, dry, obtain a kind of with broad spectrum disinfestation and the good Nutrition Soil of water retention property.
4. according to claims 2,3 with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that institute
The concentration of the aqueous hydrochloric acid solution stated is 2-3mol/L.
5. according to claims 2,3 with broad spectrum disinfestation and the good Nutrition Soil of water retention property, it is characterised in that institute
The concentration of the persulfate aqueous solution stated is 0.3-0.4mol/L.
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| CN108703038A (en) * | 2018-06-04 | 2018-10-26 | 山西省农业科学院果树研究所 | A kind of cultivation of fruit tree Nutrition Soil and preparation method thereof |
| CN110669527A (en) * | 2019-10-31 | 2020-01-10 | 安徽省农业科学院农业工程研究所 | Preparation method of special composite water-retaining agent for apocarya |
| CN114894930A (en) * | 2022-04-28 | 2022-08-12 | 浙江师范大学 | Method for detecting content of alkylphenol ethoxylates in textile by high performance liquid chromatography |
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| CN110669527A (en) * | 2019-10-31 | 2020-01-10 | 安徽省农业科学院农业工程研究所 | Preparation method of special composite water-retaining agent for apocarya |
| CN114894930A (en) * | 2022-04-28 | 2022-08-12 | 浙江师范大学 | Method for detecting content of alkylphenol ethoxylates in textile by high performance liquid chromatography |
| CN114894930B (en) * | 2022-04-28 | 2023-10-20 | 浙江师范大学 | Method for detecting alkylphenol ethoxylate content in textile by high performance liquid chromatography |
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