CN106376582A - Rotenone water dispersible granule and preparation method thereof - Google Patents
Rotenone water dispersible granule and preparation method thereof Download PDFInfo
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- CN106376582A CN106376582A CN201610771654.3A CN201610771654A CN106376582A CN 106376582 A CN106376582 A CN 106376582A CN 201610771654 A CN201610771654 A CN 201610771654A CN 106376582 A CN106376582 A CN 106376582A
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- rotenone
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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
- A01N43/90—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
-
- 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
- A01N25/02—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 liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
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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)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a rotenone water dispersible granule and a preparation method thereof. The rotenone water dispersible granule comprises the following components in percentage by weight: 10 to 90% of powdery rotenone, preferably 65%; 1 to 4% of wetting agent, preferably 2.5%; 2 to 7% of dispersant, preferably 5%; 1 to 4% of binder, preferably 2%; 2 to 5% of disintegrating agent, preferably 3%; 2 to 5% of suspending agent, preferably 3%; 3 to 6% of stabilizing agent, preferably 4%; and a carrier being added to 100%. The shortages that the conventional granule can generate dusts, the heat storage decomposition rate is high, and the generation of precipitate and blocks during the storage process is easy are overcome. The dust drifting is little when the provided rotenone water dispersible granule is used and transported, the loss and environmental pollution are avoided; the content of effective components is high, the granule is convenient to package, the storage and transportation cost is saved; the stability in storage and transportation is high; the phenomenon of layering, precipitation, and agglomeration during storage and transportation is avoided; furthermore, the granule is user-friendly, and can be rapidly disintegrated by adding the granule into water; and the dispersibility and suspension percentage are good.
Description
Technical field
The present invention usually belongs to agricultural pesticide field, and more particularly, to rotenone water dispersible granules and its
Preparation method.
Background of invention
Rotenone is a kind of insecticide, molecular formula C23H22O6.It is present in Tropical Asian and subtropical zone area produced pulse family trifoliate jewelvine
In platymiscium root, also contain in some Chinese herbal medicines such as wayaka yambean seed, thickfruit millettia seed or fruit, leatherleaf millettia root.Rotenone widely exists
In the root skin portion of plant, toxicology is a kind of very strong material of specificity, to insect especially cabbage caterpillar, diamondback moth
With aphid, there is strong tagging and two kinds of effects of stomach toxicity.The research of early stage shows that the mechanism of action of rotenone mainly affects elder brother
The respiration of worm, a certain composition mainly and nadh dehydrogenase and ubiquinone between is had an effect.Rotenone makes pest cell
Electron transport chain be suppressed, finally make insect cannot get energy supply, Ran Houhang thus reducing biological internal ATP level
Move sluggishness, benumb and slowly death.
Water dispersible granules, also known as dry suspending agent or grain type wettable powder, once putting in water, can be disintegrated quickly, dividing
Dissipate, form the granular preparation of the solid-liquid dispersing system of higher suspension.Water dispersible granules are a kind of agricultural chemicals of the exploitation eighties in last century
Novel form, because its security is good, without organic solvent, no dust, pack, transport, easy to use the advantages of developed rapidly.
As an important development direction of novel agrochemical environmental protection formulation, the agricultural chemicals that water dispersible granules have become recent domestic is leading
Formulation.Domestic enterprise is very high in the exploitation registration of water dispersible granules and popularization practical enthusiasm.Water dispersible granules are that one kind enters
The graininess formulation of the solid-liquid dispersing system being dispersed into higher suspension can be disintegrated rapidly after water, do not use organic solvent, active ingredient
Content up to 50%～90%, dispersion, suspension stability are good, suspensibility up to more than 90%, the grain fineness after dispersion reaches 8～
10 microns, drug effect and commodity performance good.Pesticide active ingredient is not readily dissolved in the agricultural chemicals product that water and organic solvent, fusing point are more than 70 DEG C
Plant and be suitable for being processed into water dispersible granules.
Although extensively water dispersible granules are applied to various agricultural chemicals, with regard to the water-dispersible grain of rotenone both at home and abroad
Agent rarely has report.Chinese patent application CN 101519475A discloses a kind of rotenone/carboxymethyl chitosan grafted branch castor oil acid
The preparation method of aqueous nanoparticle powder preparation, but the method depends on wherein disclosed carboxymethyl chitosan grafted branch castor oil
Acid copolymer.It is multiple with rotenone that Chinese patent application CN 101971830A and CN 101971833A discloses chlorine this formamide of worm
Join disinsection water dispersion granules with and preparation method thereof, this water dispersible granules wettability is good, the advantages of disintegration rate is fast.However, this
Two pieces patent all relates to compound insecticidal water dispersible granules, therefore needs to consider two in the design process of water dispersible granules simultaneously
Plant the activity of active ingredient.Additionally, these water dispersible granules produce dust, the inconvenience of suspending agent packed and transported, it is heavy that storage is also easy to produce
The shortcomings of shallow lake, caking, poor fluidity, viscous wall.
There is still a need for being specifically designed for the water dispersible granules that rotenone designs and overcomes disadvantages mentioned above in this area.
Content of the invention
The technical problem to be solved in the present invention
The rotenone water dispersible granules of prior art need by means of specific carrier or need the other insecticide of joint
Use, these water dispersible granules produce dust, suspending agent packed and transported inconvenience, storage be also easy to produce precipitation, caking, poor fluidity,
The shortcomings of viscous wall.
The technical solution used in the present invention
The invention provides a kind of rotenone water dispersible granules, it comprises the various components of following percentage by weight：
In one embodiment, described powdery rotenone is selected from rotenone root powder and rotenone crystal powder.
In one embodiment, described wetting agent be selected from wetting agent -20, sodium lignin sulphate, lauryl sodium sulfate,
And Nekal BX.
In one embodiment, described dispersant is selected from dispersant D909S, dispersant -25, dispersant -30, aryl phenol
APEO, alkylpolyoxyethylene phosphate and sulfuric ester.
In one embodiment, described binding agent is selected from high molecular weight polyethylene glycol, polyvinyl alcohol, hydroxymethyl cellulose
With sulfuric acid magnalium.
In one embodiment, described carrier is kaolin.
In one embodiment, described disintegrant is selected from disintegrant wgwin D323 and D326, calcium oxide, anhydrous slufuric acid
Sodium, sodium oxide molybdena and bentonite.
In one embodiment, described suspending agent is selected from and reaches profit pesticide dispersing agent 600C and polycarboxylic acid salt.
In one embodiment, described stabilizer is selected from disodium hydrogen phosphate, succinic acid and borax.
The technique effect of the present invention
The novel form that the rotenone water dispersible granules of the present invention grow up on the basis of wettable powder and suspending agent,
Have the characteristics that：
1. good fluidity is it is easy to measure；
2. no dust drift when using and shifting, it is to avoid waste and reduce the pollution to environment；
3. active constituent content is high, is easy to packaging and saves accumulating expense；
4. accumulating is stably well, it is to avoid suspending agent was layered in the accumulating phase, the restriction of precipitation and caking, phenomenon；
5. easy to use, it is watered and can be disintegrated rapidly during dilution, dispersiveness and suspensibility are good.
Specific embodiment
In order to make it easy to understand, providing following term and description.In the case of a conflict, it is defined by the definition of the present invention.
As used herein, term " powdery rotenone " refers to the rotenone of the powder of drying.Usually, powdery trifoliate jewelvine
The rotenone content of ketone is 10-99% and any numerical value therebetween, preferably 99%, 98%, 97%, 90% etc..This area
Technical staff understands powdery rotenone it is of course possible to containing a certain amount of impurity, such as 1%-50%, such as 5%, 10%, 20%
Etc., as long as described powdery rotenone can be applied to the present invention.In one embodiment, powdery rotenone is rotenone root
Powder and rotenone crystal powder, and above-mentioned rotenone content is equally applicable to rotenone root powder and rotenone crystal powder.
As used herein, term " wetting agent " refers to make solid material be more easy to the material being soaked in water.Wetting agent
By reducing surface tension or interfacial tension, allow the water to be deployed on solid material surface, or penetrate its surface, and solids
Material wetting.In one embodiment, described wetting agent be selected from wetting agent -20, sodium lignin sulphate, lauryl sodium sulfate,
And Nekal BX.
As used herein, " dispersant " is to promote material particles to be dispersed in medium, forms stable suspension
Medicament.In one embodiment, described dispersant is selected from dispersant D909S, dispersant -25, dispersant -30, aryl phenol
APEO, alkylpolyoxyethylene phosphate and sulfuric ester.
As used herein, " disintegrant " refers to eliminate the adhesion producing because of adhesive or high compression, from
And make the material that tablet disintegrates in water.In one embodiment, described disintegrant be selected from disintegrant wgwin D323 and
D326, calcium oxide, anhydrous sodium sulfate, sodium oxide molybdena and bentonite.
As used herein, stabilizer refers to increase the compound of the stability of solution, colloid, solid, mixture.?
In one embodiment, described stabilizer is selected from disodium hydrogen phosphate, succinic acid and borax.
In one embodiment, described binding agent is selected from high molecular weight polyethylene glycol, polyvinyl alcohol, hydroxymethyl cellulose
With sulfuric acid magnalium.
The preparation method of rotenone water dispersible granules is as follows：Add other components in rotenone active compound, through air-flow crushing or
Ultra-fine grinding, fineness reaches 185-300 mesh, obtains wettable powder, is then granulated, wherein prilling process includes but is not limited to
Rotary table granulation, extruder grain, adjustment mixing granulation, thermopnore granulation and compression granulation.
Used in the present invention, material is all that business can reach, skilled artisan would appreciate that the realization of the present invention
It is not limited to these sources.
Embodiment
Material and method
Rotenone active compound：Purchased from Shilennonghua Tech Development Co., Ltd., Guangxi；Purity 95%
Lauryl sodium sulfate：Suzhou Yuan Tairun Chemical Co., Ltd.；
Alkylpolyoxyethylene phosphate C1618：Hai'an petrochemical plant
Kaolin：Anji County triumph bentonite factory
Bentonite：Anji County triumph bentonite factory
Reach profit pesticide dispersing agent 600C：Shenzhen Langtai Biotechnology Technology Co., Ltd.
Succinic acid：Shanghai Ya Nong pesticide chemical Co., Ltd
Powdered polyvinyl alcohol：Shanghai Ying Jia industry development Co., Ltd
Rotenone water dispersible granules performance indications measure
Active constituent content：Sample acetone solution, rotenone content with equipped with HypersilODS (5m, 250mm ×
4mm) the rp-hplc determination of chromatographic column and UV-detector.Determine optimal liquid chromatographic detection condition be：
Detection wavelength 290nm；Mobile phase, volume ratio is 60:40 acetonitrile/water mixed liquor, flow velocity 1mL/min, sample size 10 μ L.
Thermal storage stability is tested：Test sample is stored 14 days under the conditions of air-tight state (54 ± 2) DEG C, and inspection preparation is each
Item physical and chemical mutagenesis.
Dust is tested：Carry out by Chinese graininess agricultural chemicals dust assay method standard (GB/T 30360-2013).
Water-dispersible granules WDG disintegrative measures：To tool plug graduated cylinder (the interior height of the 100mL containing 90ral distilled water
22.5cm, internal diameter 28ram) in, add sample particle (0.5g) at 25 DEG C, clamp the middle part of graduated cylinder afterwards, clog nozzle, with
The speed of 8r/min, around central rotation, until sample is disintegrated in water completely, calculates disintegration time.
Embodiment 1：Prepared by rotenone water dispersible granules
Take rotenone active compound 10g, lauryl sodium sulfate 2.5g；Alkylpolyoxyethylene phosphate C1618 5g；
Powdered polyvinyl alcohol 2g；Bentonite reaches profit 3g；Reach profit pesticide dispersing agent 600C 3g, succinic acid 4g；Kaolin 69.5g；Blended
Afterwards, pulverize through airslide disintegrating mill, make pulvis (250 mesh), but extruder grain, obtain 10% rotenone water dispersible granules (sample
Product 1).
Take rotenone active compound 30g, lauryl sodium sulfate 2.5g；Alkylpolyoxyethylene phosphate C1618 5g；
Powdered polyvinyl alcohol 2g；Bentonite reaches profit 3g；Reach profit pesticide dispersing agent 600C 3g, succinic acid 4g；Kaolin 49.5g；Blended
Afterwards, pulverize through airslide disintegrating mill, make pulvis (250 mesh), but extruder grain, obtain 30% rotenone water dispersible granules (sample
Product 2).
Take rotenone active compound 50g, lauryl sodium sulfate 2.5g；Alkylpolyoxyethylene phosphate C1618 5g；
Powdered polyvinyl alcohol 2g；Bentonite reaches profit 3g；Reach profit pesticide dispersing agent 600C 3g, succinic acid 4g；Kaolin 29.5g；Blended
Afterwards, pulverize through airslide disintegrating mill, make pulvis (250 mesh), but extruder grain, obtain 50% rotenone water dispersible granules (sample
Product 3).
Take rotenone active compound 65g, lauryl sodium sulfate 2.5g；Alkylpolyoxyethylene phosphate C1618 5g；
Powdered polyvinyl alcohol 2g；Bentonite reaches profit 3g；Reach profit pesticide dispersing agent 600C 3g, succinic acid 4g；Kaolin 14.5g；Blended
Afterwards, pulverize through airslide disintegrating mill, make pulvis (250 mesh), but extruder grain, obtain 65% rotenone water dispersible granules (sample
Product 4).
Take rotenone active compound 70g, lauryl sodium sulfate 2.5g；Alkylpolyoxyethylene phosphate C1618 5g；
Powdered polyvinyl alcohol 2g；Bentonite reaches profit 3g；Reach profit pesticide dispersing agent 600C 3g, succinic acid 4g；Kaolin 9.5g；Blended
Afterwards, pulverize through airslide disintegrating mill, make pulvis (250 mesh), but extruder grain, obtain 70% rotenone water dispersible granules (sample
Product 5).
Embodiment 2：Thermal storage stability is tested
The rotenone water dispersible granules (sample 1-5) taking above-mentioned various concentration carry out thermal storage stability test.Hereafter, survey
Determine the active ingredient of each sample and make following table.All samples are carried out in triplicate, and numerical value is averaged.
Result：
Table 1：Thermal storage stability.
Relative rate of resolution is in tending to of increase typically with concentration, but the relative rate of resolution of 65% rotenone water dispersible granules
But apparently higher than other samples.
Embodiment 2：Dust is tested
Above-mentioned sample 1-5 is taken to carry out dust test, all samples are carried out in triplicate, and numerical value is averaged.Test result
As follows：
According to Chinese graininess agricultural chemicals dust assay method standard (GB/T 30360-2013) regulation, result judgement standard
As follows：
| Measured value/the mg of dust | Result judgement |
| ≤30 | Substantially no dust |
| >30 | There is dust |
Test result shows, the recipe ingredient of the present invention can be tested by dust, substantially no dust.
Embodiment 3：The impact that granularity is tested to dust
Take rotenone active compound 65g, lauryl sodium sulfate 2.5g；Alkylpolyoxyethylene phosphate C1618 5g；
Powdered polyvinyl alcohol 2g；Bentonite reaches profit 3g；Reach profit pesticide dispersing agent 600C 3g, succinic acid 4g；Kaolin 14.5g；Blended
Afterwards, pulverize through airslide disintegrating mill, make pulvis 100,150,200,250 and 300 mesh, but extruder grain, respectively obtain 65%
Rotenone water dispersible granules sample 1-5.
Above-mentioned 65% rotenone water dispersible granules sample 1-5 is taken to carry out dust test, all samples are carried out in triplicate, number
Value is averaged.Test result is as follows：
| Sample number | Dust concentration/mg |
| 1 (65%) | 35.8 |
| 2 (65%) | 30.4 |
| 3 (65%) | 32.2 |
| 4 (65%) | 28.3 |
| 5 (65%) | 37.2 |
Test result shows, can be tested by dust by the recipe ingredient of the present invention of 250 mesh, substantially no dust.
Embodiment 4：Disintegrative measures
Described in Example 3, sample 1-5 carries out dust test, and all samples are carried out in triplicate, and numerical value is averaged.
Test result is as follows：
| Sample number | Disintegration time (second) |
| 1 | 156 |
| 2 | 143 |
| 3 | 145 |
| 4 | 133 |
| 5 | 140 |
Test result shows, the recipe ingredient of the present invention has good disintegrative, wherein has best with the effect of sample 4.
Above example is exemplified with the present invention, but those skilled in the art can be without departing from spirit and scope of the invention
On the premise of modify, these are still in the protection domain of appended claims.
Claims (10)
1. a kind of rotenone water dispersible granules, it comprises the various components of following percentage by weight：
2. rotenone water dispersible granules according to claim 1, wherein said powdery rotenone is selected from rotenone root powder, fish
Rattan ketone crystal powder, rotenone crude oil dry xeraphium and derris root powder.
3. rotenone water dispersible granules according to claim 1, wherein said wetting agent is selected from wetting agent -20, lignin
Sodium sulphate, lauryl sodium sulfate and Nekal BX.
4. rotenone water dispersible granules according to claim 1, wherein said dispersant is selected from dispersant D909S, dispersion
Agent -25, dispersant -30, aryl phenol polyethenoxy ether, alkylpolyoxyethylene phosphate and sulfuric ester.
5. rotenone water dispersible granules according to claim 1, wherein said carrier is kaolin.
6. rotenone water dispersible granules according to claim 1, wherein said disintegrant is selected from disintegrant wgwin D323
With D326, calcium oxide, anhydrous sodium sulfate, sodium oxide molybdena and bentonite.
7. rotenone water dispersible granules according to claim 1, wherein said suspending agent is selected from and reaches profit pesticide dispersing agent
600C and polycarboxylic acid salt.
8. rotenone water dispersible granules according to claim 1, wherein said stabilizer is selected from disodium hydrogen phosphate, succinic acid
And borax.
9. rotenone water dispersible granules according to claim 1, binding agent is selected from high molecular weight polyethylene glycol, polyethylene
Alcohol, hydroxymethyl cellulose and sulfuric acid magnalium.
10. the preparation method of the rotenone water dispersible granules of claim 1, adds other components wherein in rotenone active compound,
Through air-flow crushing or ultra-fine grinding, fineness reaches 185-300 mesh, and preferably 250 mesh obtain wettable powder, then granulated, its
Middle prilling process includes but is not limited to rotary table granulation, extruder grain, adjustment mixing granulation, thermopnore granulation and compression granulation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610771654.3A CN106376582A (en) | 2016-08-30 | 2016-08-30 | Rotenone water dispersible granule and preparation method thereof |
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| CN201610771654.3A CN106376582A (en) | 2016-08-30 | 2016-08-30 | Rotenone water dispersible granule and preparation method thereof |
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| Publication Number | Publication Date |
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| CN106376582A true CN106376582A (en) | 2017-02-08 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106721624A (en) * | 2016-12-07 | 2017-05-31 | 重庆文洪水产品养殖有限公司 | A kind of anti-oxidant heavy property aquatic products food calling particle and preparation method thereof |
| CN108477220A (en) * | 2018-02-01 | 2018-09-04 | 鹤壁市人元生物技术发展有限公司 | A kind of aspergillus parasiticus spore composite insecticide and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104222161A (en) * | 2014-08-29 | 2014-12-24 | 广东省农业科学院植物保护研究所 | Insecticide composition as well as preparation method and application of insecticide composition |
-
2016
- 2016-08-30 CN CN201610771654.3A patent/CN106376582A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104222161A (en) * | 2014-08-29 | 2014-12-24 | 广东省农业科学院植物保护研究所 | Insecticide composition as well as preparation method and application of insecticide composition |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106721624A (en) * | 2016-12-07 | 2017-05-31 | 重庆文洪水产品养殖有限公司 | A kind of anti-oxidant heavy property aquatic products food calling particle and preparation method thereof |
| CN108477220A (en) * | 2018-02-01 | 2018-09-04 | 鹤壁市人元生物技术发展有限公司 | A kind of aspergillus parasiticus spore composite insecticide and preparation method thereof |
| CN108477220B (en) * | 2018-02-01 | 2020-05-26 | 鹤壁市人元生物技术发展有限公司 | Aspergillus parasiticus spore composite pesticide and preparation method thereof |
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Application publication date: 20170208 |