CN109673631A - A kind of environmentally friendly fluorine worm benzamide nanometer pulvis and preparation method thereof - Google Patents

A kind of environmentally friendly fluorine worm benzamide nanometer pulvis and preparation method thereof Download PDF

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Publication number
CN109673631A
CN109673631A CN201811618803.8A CN201811618803A CN109673631A CN 109673631 A CN109673631 A CN 109673631A CN 201811618803 A CN201811618803 A CN 201811618803A CN 109673631 A CN109673631 A CN 109673631A
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CN
China
Prior art keywords
fluorine worm
environmentally friendly
worm benzamide
auxiliary agent
component
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201811618803.8A
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Chinese (zh)
Inventor
张子勇
梁冰
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Nanjing Scienx Biotechnology Co Ltd
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Nanjing Scienx Biotechnology Co Ltd
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Priority to CN201811618803.8A priority Critical patent/CN109673631A/en
Publication of CN109673631A publication Critical patent/CN109673631A/en
Priority to PCT/IB2019/057429 priority patent/WO2020136451A1/en
Priority to GB2010113.5A priority patent/GB2587264B/en
Priority to GB2010112.7A priority patent/GB2585502B/en
Priority to PCT/IB2019/057428 priority patent/WO2020136450A1/en
Priority to CN201980086511.0A priority patent/CN113260257B/en
Priority to PCT/CN2019/128757 priority patent/WO2020135600A1/en
Priority to PCT/CN2019/129436 priority patent/WO2020135780A1/en
Withdrawn legal-status Critical Current

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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
    • A01N25/12Powders or granules
    • 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
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/561,2-Diazoles; Hydrogenated 1,2-diazoles

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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)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention belongs to technical field of pesticide, especially a kind of environmentally friendly fluorine worm benzamide nanometer pulvis, including active components A, the active components A is fluorine worm benzamide, further includes solvent 8-23wt%, small molecule auxiliary agent 10-25wt%, pluronic polymer less than 9-17wt% and dispersing agent water 35-52wt%.After above-mentioned formula and technique, fluorine worm benzamide nanometer pulvis nanoscale prepared by the present invention, the pesticide of same quality, the area of more pesticide granule amounts, bigger surface area and target contact is just wider, the drug effect of performance is just higher, it can be used for aviation plant protection special agent, do not generate precipitating, spray head will not be blocked;Environmental-friendly auxiliary agent is selected, does not select high poison solvent and auxiliary agent, it is more efficient, more environmentally friendly and safer, it changes in the past only with efficient, less toxic for preferred state, it is desirable that medicament is environmentally safe as the most important condition.

Description

A kind of environmentally friendly fluorine worm benzamide nanometer pulvis and preparation method thereof
Technical field
The invention belongs to technical field of pesticide, especially a kind of environmentally friendly fluorine worm benzamide nanometer pulvis and its system Preparation Method.
Background technique
The suckings pest such as aphid, plant hopper, thrips, scale insect are short with the breeding cycle, breeding amount is big, generation overlap The features such as obvious, are easy to develop drug resistance.Used due to year after year a large amount of, above-mentioned pest for medicaments such as imidacloprid, Acetamiprids Through generating serious resistance.
Japanese pesticide company in 1998 develop first act on the compound Flubendiamide of target ryanodine receptor after, E.I.Du Pont Company on its basis, based on Flubendiamide, successively developed new a kind of lead compound chlorine worm benzoyl Amine.Since these two types of compound structures are similar, the mechanism of action is identical, broad-spectrum high-efficiency and low-toxicity, and major research institution carries out ryania The research initiative of receptor insecticide forms several insecticides: phthalic diamides, adjacent formamido benzamides, two Amides, adjacent heterocycle benzamides agrochemical.
103858899 A of Chinese invention patent application CN discloses a kind of containing spiral shell worm ethyl ester and amide insecticides Composition pesticide, effective component are that (A) spiral shell worm ethyl ester and (B) are selected from one of amide insecticides.The wherein matter of A and B It is 1~80% that amount percentage, which is content of 1~80: 80~1, the A and B in compound preparation,.Compound pesticide composition of the present invention is adopted Missible oil, suspending agent, wettable powder, water dispersible granules, water and milk can be prepared into method known in those skilled in the art The dosage forms such as agent.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of Environmental security and efficient fluorine worm benzamide nano powders Agent and preparation method thereof.
In order to solve the above technical problems, a kind of environmentally friendly fluorine worm benzamide nanometer pulvis of the invention, including Active components A, the active components A be fluorine worm benzamide, further include solvent 8-23wt%, small molecule auxiliary agent 10-25wt%, Pluronic polymer is less than 9-17wt% and dispersing agent water 35-52wt%.
Preferably, the solvent selects one or both of acetone or cyclohexanone.
Preferably, the biodegradable small molecule auxiliary agent of the small molecule selection of auxiliary, including anionic surface activity Agent or nonionic surface active agent.
Preferably, the ionic surfactant includes carboxylate, the sulphur for the straight chained alkyl that different carbon atom numbers are constituted Hydrochlorate, sulfate, the nonionic surface active agent include straight chained alkyl ether, the ester, amide that different carbon atom numbers are constituted Polyoxyethylene ether, at least two mixture in the biodegradable above-mentioned surfactant of small molecule selection of auxiliary, The HLB value position 12-15 of the small molecule auxiliary agent, dosage 10-25%.
Preferably, the pluronic polymer selects water soluble polymer auxiliary agent, including water-soluble macromolecule and its spreads out Biology or synthesis macromolecule.
Preferably, the water-soluble macromolecule and its derivative include dextrin, cyclodextrin, water soluble starch, oxidation Starch, carboxymethyl starch, modified starch, carboxymethyl cellulose, hydroxyethyl hydroxypropyl base cellulose;Carboxymethyl chitosan, modified melon That glue, Tea Saponin, the synthesis macromolecule select polyvinyl alcohol, Sodium Polyacrylate, polyacrylamide, polypyrrole alkanone, polyphenyl Ethylene-maleic acid sodium, the water soluble polymer selection of auxiliary are one such or several.
The invention also discloses a kind of environmentally friendly fluorine worm benzamide nanometer pulvis preparation method, the preparation methods Include the following steps,
(1) a certain amount of pesticide original medicine is dissolved in solvent or in the mixed solvent, be configured to close to saturated solution, referred to as component A;
(2) a certain amount of pluronic polymer is dissolved in water, stirs, is configured to certain density aqueous solution, referred to as group Divide B;
(3) a certain amount of small molecule auxiliary agent is added in component B, stirring is configured to composite assistant solution, referred to as component C;
(4) under agitation, it by the pesticide solution, that is, component A, instills in composite assistant solution, that is, component C, control is added dropwise Speed makes it not generate precipitating, and keeps solution transparent, becomes component D;
(5) component D is spray-dried, obtains target product.
Preferably, the pesticide original medicine in the step (1) includes active components A, and the active components A is fluorine worm benzoyl Amine.
Preferably, the pluronic polymer in the step (2) be selected from dextrin, cyclodextrin, water soluble starch, oxidized starch, Carboxymethyl starch, modified starch, carboxymethyl cellulose, hydroxyethyl hydroxypropyl base cellulose, carboxymethyl chitosan, modified guar, Tea Saponin, the synthesis macromolecule select polyvinyl alcohol, Sodium Polyacrylate, polyacrylamide, polypyrrole alkanone, polystyrene- One or more of maleic acid sodium.
Preferably, the small molecule auxiliary agent in the step (3) is selected from carboxylate, sulfonate, sulfate, different carbon atom numbers The straight chained alkyl ether of composition, ester, amide polyoxyethylene ether at least two, the HLB value position 12- of the small molecule auxiliary agent 15, dosage 10-25%.
After above-mentioned formula and technique, fluorine worm benzamide nanometer pulvis nanoscale prepared by the present invention, same quality Pesticide, the area of more pesticide granule amounts, bigger surface area and target contact is just wider, and the drug effect of performance is just more Height, can be used for aviation plant protection special agent, not generate precipitating, will not block spray head;Environmental-friendly auxiliary agent is selected, is not selected High poison solvent (benzene, toluene, dimethylbenzene, methanol) and auxiliary agent (nonylphenol polyoxyethylene ether), it is more efficient, more environmentally friendly and safer, It changes in the past only with efficient, less toxic for preferred state, it is desirable that medicament is environmentally safe as the most important condition.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but these embodiments are not Limiting the scope of the invention." one embodiment " or " embodiment " referred to herein, which refers to, may be included in the present invention at least A particular feature, structure, or characteristic in one implementation.In the present specification different places occur " in one embodiment In " the same embodiment not is referred both to, nor the individual or selective embodiment mutually exclusive with other embodiments.
Wt% in the present invention refers to that each raw material accounts for the mass percent of total mass of raw material.
Embodiment 1
A kind of environmentally friendly fluorine worm benzamide nanometer pulvis, including active components A, the active components A are fluorine worm Benzamide, active constituent 10wt% further include solvent 15wt%, small molecule auxiliary agent 16wt%, pluronic polymer 14wt%, divide Powder water 45wt%.
Wherein, solvent selects acetone.
Wherein, the biodegradable small molecule auxiliary agent of small molecule selection of auxiliary, including anionic surfactant or non- Ionic surfactant, ionic surfactant include carboxylate, the sulfonic acid for the straight chained alkyl that different carbon atom numbers are constituted Salt, nonionic surface active agent includes the polyoxyethylene ether of the straight chained alkyl ether of different carbon atom numbers compositions, ester, amide, small The HLB value position 12-15 of molecule auxiliary agent, dosage 10%.
Wherein, pluronic polymer selects water soluble polymer auxiliary agent, including water-soluble macromolecule and its derivative, day Right water soluble polymer and its derivative select dextrin, cyclodextrin and water soluble starch.
Environmentally friendly fluorine worm benzamide nanometer pulvis preparation method in the present embodiment includes the following steps,
(1) pesticide original medicine is dissolved in solvent or in the mixed solvent, be configured to close to saturated solution (pesticide active ingredient Content will be less than the content in final nano-powder preparation), referred to as component A;
(2) pluronic polymer is dissolved in water, stirs, is configured to certain density aqueous solution, referred to as component B;
(3) small molecule auxiliary agent is added in component B, stirring is configured to composite assistant solution, referred to as component C;
(4) under agitation, it by the pesticide solution, that is, component A, instills in composite assistant solution, that is, component C, control is added dropwise Speed makes it not generate precipitating, and keeps solution transparent, becomes component D;
(5) component D is spray-dried, obtains target product.
Embodiment 2
A kind of environmentally friendly fluorine worm benzamide nanometer pulvis, including active components A, the active components A are fluorine worm The mass fraction of benzamide, active constituent is 9wt%, further includes solvent 21wt%, small molecule auxiliary agent 13wt%, polymeric retention aid Agent 17wt% and dispersing agent water 40wt%.
Wherein, solvent selects cyclohexanone.
Wherein, the biodegradable small molecule auxiliary agent of small molecule selection of auxiliary, including anionic surfactant, ion Type surfactant includes carboxylate, sulfonate, the sulfate for the straight chained alkyl that different carbon atom numbers are constituted, small molecule auxiliary agent HLB value position 12-15, dosage 25%.
Wherein, pluronic polymer selects water soluble polymer auxiliary agent, including water-soluble macromolecule and its derivative, day Right water soluble polymer and its derivative include carboxymethyl chitosan, modified guar, Tea Saponin.
Environmentally friendly fluorine worm benzamide nanometer pulvis preparation method in the present embodiment includes the following steps,
(1) pesticide original medicine is dissolved in solvent or in the mixed solvent, be configured to close to saturated solution (pesticide active ingredient Content will be less than the content in final nano-powder preparation), referred to as component A;
(2) pluronic polymer is dissolved in water, stirs, is configured to certain density aqueous solution, referred to as component B;
(3) small molecule auxiliary agent is added in component B, stirring is configured to composite assistant solution, referred to as component C;
(4) under agitation, it by the pesticide solution, that is, component A, instills in composite assistant solution, that is, component C, control is added dropwise Speed makes it not generate precipitating, and keeps solution transparent, becomes component D;
(5) component D is spray-dried, obtains target product.
Embodiment 3
A kind of environmentally friendly fluorine worm benzamide nanometer pulvis, including active components A, the active components A are fluorine worm Benzamide, active constituent account for 8wt%, further include solvent 18wt%, small molecule auxiliary agent 14wt%, pluronic polymer 9wt% and Dispersing agent water 51wt%.
Wherein, solvent selects acetone and cyclohexanone to mix according to volume ratio 1: 1.
Wherein, the biodegradable small molecule auxiliary agent of small molecule selection of auxiliary, including nonionic surface active agent, it is non-from Subtype surfactant includes the polyoxyethylene ether of the straight chained alkyl ether of different carbon atom numbers compositions, ester, amide, small molecule auxiliary agent HLB value position 12-15, dosage 10-25%.
Wherein, pluronic polymer selects water soluble polymer auxiliary agent, including synthesis macromolecule, and synthesis macromolecule selects poly- second Enol, Sodium Polyacrylate, polyacrylamide, polypyrrole alkanone, polystyrene-maleic acid sodium.
Environmentally friendly fluorine worm benzamide nanometer pulvis preparation method in the present embodiment includes the following steps,
(1) pesticide original medicine is dissolved in solvent or in the mixed solvent, be configured to close to saturated solution (pesticide active ingredient Content will be less than the content in final nano-powder preparation), referred to as component A;
(2) pluronic polymer is dissolved in water, stirs, is configured to certain density aqueous solution, referred to as component B;
(3) small molecule auxiliary agent is added in component B, stirring is configured to composite assistant solution, referred to as component C;
(4) under agitation, it by the pesticide solution, that is, component A, instills in composite assistant solution, that is, component C, control is added dropwise Speed makes it not generate precipitating, and keeps solution transparent, becomes component D;
(5) component D is spray-dried, obtains target product.
The above description is merely a specific embodiment, and scope of protection of the present invention is not limited thereto, any ripe Know those skilled in the art in the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of, should all contain Lid is within protection scope of the present invention.Therefore, the protection scope that protection scope of the present invention should be defined with claim Subject to.

Claims (10)

1. a kind of environmentally friendly fluorine worm benzamide nanometer pulvis, it is characterised in that: including active components A, it is described activity at Dividing A is fluorine worm benzamide, further includes solvent 8-23wt%, small molecule auxiliary agent 10-25wt%, pluronic polymer less than 9- 17wt% and dispersing agent water 35-52wt%.
2. a kind of environmentally friendly fluorine worm benzamide nanometer pulvis according to claim 1, it is characterised in that: described molten One or both of acetone or cyclohexanone are selected in agent.
3. a kind of environmentally friendly fluorine worm benzamide nanometer pulvis according to claim 1, it is characterised in that: described small The biodegradable small molecule auxiliary agent of molecule selection of auxiliary, including anionic surfactant or non-ionic surfactant Agent.
4. a kind of environmentally friendly fluorine worm benzamide nanometer pulvis according to claim 3, it is characterised in that: it is described from Subtype surfactant includes carboxylate, sulfonate, the sulfate for the straight chained alkyl that different carbon atom numbers are constituted, the nonionic Type surfactant includes the polyoxyethylene ether of the straight chained alkyl ether of different carbon atom numbers compositions, ester, amide, described biological to drop At least two mixture in the above-mentioned surfactant of small molecule selection of auxiliary of solution, the HLB value position of the small molecule auxiliary agent 12-15, dosage 10-25%.
5. a kind of environmentally friendly fluorine worm benzamide nanometer pulvis according to claim 1, it is characterised in that: the height Molecule selection of auxiliary water soluble polymer auxiliary agent, including water-soluble macromolecule and its derivative or synthesis macromolecule.
6. a kind of environmentally friendly fluorine worm benzamide nanometer pulvis according to claim 5, it is characterised in that: the day Right water soluble polymer and its derivative include dextrin, cyclodextrin, water soluble starch, oxidized starch, carboxymethyl starch, modified shallow lake Powder, carboxymethyl cellulose, hydroxyethyl hydroxypropyl base cellulose;Carboxymethyl chitosan, modified guar, Tea Saponin, the synthesis are high Molecule selects polyvinyl alcohol, Sodium Polyacrylate, polyacrylamide, polypyrrole alkanone, polystyrene-maleic acid sodium, described Water soluble polymer selection of auxiliary is one such or several.
7. a kind of environmentally friendly fluorine worm benzamide nanometer pulvis preparation method, it is characterised in that: the preparation method includes Following steps,
(1) a certain amount of pesticide original medicine is dissolved in solvent or in the mixed solvent, be configured to close to saturated solution, referred to as component A;
(2) a certain amount of pluronic polymer is dissolved in water, stirs, is configured to certain density aqueous solution, referred to as component B;
(3) a certain amount of small molecule auxiliary agent is added in component B, stirring is configured to composite assistant solution, referred to as component C;
(4) under agitation, it by the pesticide solution, that is, component A, instills in composite assistant solution, that is, component C, controls rate of addition, So that it is not generated precipitating, and keep solution transparent, becomes component D;
(5) component D is spray-dried, obtains target product.
8. a kind of environmentally friendly fluorine worm benzamide nanometer pulvis preparation method according to claim 7, feature exist In: the pesticide original medicine in the step (1) includes active components A, and the active components A is fluorine worm benzamide.
9. a kind of environmentally friendly fluorine worm benzamide nanometer pulvis preparation method according to claim 7, feature exist Dextrin is selected from: pluronic polymer in the step (2), cyclodextrin, water soluble starch, oxidized starch, carboxymethyl starch, is changed Property starch, carboxymethyl cellulose, hydroxyethyl hydroxypropyl base cellulose, carboxymethyl chitosan, modified guar, Tea Saponin, the conjunction At in macromolecule selection polyvinyl alcohol, Sodium Polyacrylate, polyacrylamide, polypyrrole alkanone, polystyrene-maleic acid sodium One or more.
10. a kind of environmentally friendly fluorine worm benzamide nanometer pulvis preparation method according to claim 7, feature exist In: the small molecule auxiliary agent in the step (3) is selected from the straight chain alkane that carboxylate, sulfonate, sulfate, different carbon atom numbers are constituted Base ether, ester, amide polyoxyethylene ether at least two, the HLB value position 12-15 of the small molecule auxiliary agent, dosage 10- 25%.
CN201811618803.8A 2018-12-28 2018-12-28 A kind of environmentally friendly fluorine worm benzamide nanometer pulvis and preparation method thereof Withdrawn CN109673631A (en)

Priority Applications (8)

Application Number Priority Date Filing Date Title
CN201811618803.8A CN109673631A (en) 2018-12-28 2018-12-28 A kind of environmentally friendly fluorine worm benzamide nanometer pulvis and preparation method thereof
PCT/IB2019/057429 WO2020136451A1 (en) 2018-12-28 2019-09-04 Method for preparing miscible nano-pesticide suspension
GB2010113.5A GB2587264B (en) 2018-12-28 2019-09-04 Method for preparing miscible nanosuspension
GB2010112.7A GB2585502B (en) 2018-12-28 2019-09-04 Miscible nanosuspension
PCT/IB2019/057428 WO2020136450A1 (en) 2018-12-28 2019-09-04 Miscible nano-sized pesticide suspension
CN201980086511.0A CN113260257B (en) 2018-12-28 2019-12-26 Nano pesticide preparation and preparation method thereof
PCT/CN2019/128757 WO2020135600A1 (en) 2018-12-28 2019-12-26 Nano pesticide formulation and preparation method therefor
PCT/CN2019/129436 WO2020135780A1 (en) 2018-12-28 2019-12-27 Nano agro-chemical preparation, and preparation method therefor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811618803.8A CN109673631A (en) 2018-12-28 2018-12-28 A kind of environmentally friendly fluorine worm benzamide nanometer pulvis and preparation method thereof

Publications (1)

Publication Number Publication Date
CN109673631A true CN109673631A (en) 2019-04-26

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020135780A1 (en) * 2018-12-28 2020-07-02 南京善思生物科技有限公司 Nano agro-chemical preparation, and preparation method therefor
WO2020136451A1 (en) * 2018-12-28 2020-07-02 张子勇 Method for preparing miscible nano-pesticide suspension

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020135780A1 (en) * 2018-12-28 2020-07-02 南京善思生物科技有限公司 Nano agro-chemical preparation, and preparation method therefor
WO2020136451A1 (en) * 2018-12-28 2020-07-02 张子勇 Method for preparing miscible nano-pesticide suspension
WO2020135600A1 (en) * 2018-12-28 2020-07-02 南京善思生物科技有限公司 Nano pesticide formulation and preparation method therefor
GB2587264A (en) * 2018-12-28 2021-03-24 Zhang Ziyong Method for preparing miscible nano-pesticide suspension
CN113260257A (en) * 2018-12-28 2021-08-13 南京善思生物科技有限公司 Nano pesticide preparation and preparation method thereof
CN113260257B (en) * 2018-12-28 2022-09-06 南京善思生物科技有限公司 Nano pesticide preparation and preparation method thereof
GB2587264B (en) * 2018-12-28 2022-11-09 Zhang Ziyong Method for preparing miscible nanosuspension

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Application publication date: 20190426