CN106818727A - A kind of emamectin-benzoate mite killing suspending agent for suppressing chitin synthesis and preparation method thereof - Google Patents
A kind of emamectin-benzoate mite killing suspending agent for suppressing chitin synthesis and preparation method thereof Download PDFInfo
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- CN106818727A CN106818727A CN201611202582.7A CN201611202582A CN106818727A CN 106818727 A CN106818727 A CN 106818727A CN 201611202582 A CN201611202582 A CN 201611202582A CN 106818727 A CN106818727 A CN 106818727A
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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
- A01N25/02—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
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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
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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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/34—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the groups, e.g. biuret; Thio analogues thereof; Urea-aldehyde condensation products
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Abstract
A kind of emamectin-benzoate mite killing suspending agent for suppressing chitin synthesis, it is characterised in that it is prepared from by following raw material：Emamectin benzoate, methyl alcohol, phosphoric acid solution, toluene, isopropyl acetate, fatty acid monoglyceride, benzoic acid, n-hexane, diflubenzuron, ethyl acetate, dichloromethane, acetone, laruyl alcohol sulfosuccinate disodium, polyvinyl alcohol, xanthans, shitosan, acetic acid, polyethylene glycol, atoleine, Geniposide, citric acid dibutyl naphthalenesulfonic acid calcium, palmitic acid formicester, triethanolamine, appropriate deionized water.Mite killing suspending agent of the invention can efficiently lure acarid, acarid is effectively killed, with excellent synergistic effect, acaricidal field dosage is reduced, residues of pesticides and the harm to beneficial organism can be effectively reduced, while reducing cost accounting and mitigating the pollution to environment.
Description
Technical field
The invention belongs to agricultural pesticide field, and in particular to a kind of emamectin benzoate benzene first of suppression chitin synthesis
Hydrochlorate mite killing suspending agent and preparation method thereof.
Background technology
It is current main to use chemical pesticide control agricultural pest, but over time, the drawbacks of chemical pesticide by
Gradually it is exposed, of particular concern is the rampant and resistance problem mad again of residues of pesticides, insect, these problems promotes people to open
Beginning finds the substitute of chemical pesticide.AVM is that antibioticses desinsection kills full mite agent, belongs to biological source insecticide, with chemistry
Unlike agricultural chemical insecticide, AVM mainly by disturbing insect nervous physiology activity, stimulates release GABA,
And aminobutyric acid has inhibitory action to the nerve conduction of arthropod, mite class adult, nymph and insect larvae and AVM connect
There is paralysis symptom after touch, inertia, do not take food, it is dead after 2~4 days.AVM is to insect predator and insect parasite
Though there is direct action of contace poison, because plant surface residual is few, therefore to the damage very little of beneficial insect.AVM is in soil by soil
Absorption will not be moved, and can be decomposed by the microorganisms, thus in the environment without cumulative function.Due to not causing insect to take off rapidly
Water, AVM lethal effect is more slow.
Author Chen Fuliang exists《The development of the avermectin micro-emulsion containing organosilicon auxiliary agent》In one text, with 7% Avermectin
Element, 6% cyclohexanone, 4% dimethyl sulfoxide (DMSO), 5% organosilicon auxiliary agent Silwet408 and balance of water, are obtained AVM micro-
Emulsion；Addition organosilicon auxiliary agent can not only significantly reduce liquid surface tension and improve liquid blade surface wetting,
Ability is opened up, increases the expanding area of liquid, and liquid can be made to enter hidden close insect hiding place, and promote plant leaf surface pair
The absorption of active ingredient and enter epidermis, extend its lasting period；But active ingredient is single Avermectin in the microemulsion
Element, its Insecticiding-miticiding is inefficient, and lethal effect is slow.
The content of the invention
It is an object of the invention to provide the emamectin benzoate benzene of a kind of efficient and lasting suppression chitin synthesis
Formates mite killing suspending agent and preparation method thereof.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of emamectin-benzoate mite killing suspending agent for suppressing chitin synthesis, it is characterised in that it is by as follows
The raw material of weight portion is prepared from：Emamectin benzoate 6-8 parts, methyl alcohol 120-150 parts, phosphoric acid solution 30-40 parts, toluene
200-250 parts, isopropyl acetate 60-70 parts, fatty acid monoglyceride 2-3 parts, benzoic acid 12-15 parts, n-hexane 180-200
Part, diflubenzuron 4-5 parts, ethyl acetate 50-60 parts, dichloromethane 40-50 parts, acetone 80-100 parts, laruyl alcohol sulfosuccinic acid
1-2 parts of ester disodium, polyvinyl alcohol 10-12 parts, xanthans 3-4 parts, shitosan 18-20 parts, acetic acid 4-5 parts, polyethylene glycol 2-3
Part, atoleine 80-100 parts, Geniposide 4-5 parts, 0.5-1 parts of citric acid dibutyl naphthalenesulfonic acid calcium, 2-3 parts of palmitic acid formicester,
Triethanolamine 3-4 parts, appropriate deionized water.
The emamectin-benzoate mite killing suspending agent of described suppression chitin synthesis, it is characterised in that its
It is prepared from by following steps：
（1）At room temperature, emamectin benzoate is added in 2/3 methyl alcohol, is stirred to being completely dissolved, be slowly added dropwise phosphoric acid molten
The mixed solution that liquid is configured with remaining methyl alcohol, continues to mix 1-2h after completion of dropping；1/2 toluene is added, continues mixed
Conjunction stirring 1-2h, is transferred them in ice-water bath, continues to mix 5-6h, and centrifugation, precipitation is used and pre-cooled to 0 DEG C
Remaining toluene wash 2-3 time, be vacuum dried；Product after vacuum drying is added to equivalent to emamectin benzoate weight
Measure in the deionized water of 3-4 times of part, stirring dissolves it, add isopropyl acetate, regulation system PH is 8-9, mixes 30-
3-4h is stood after 40min, organic phase is separated；Fatty acid monoglyceride is added in organic phase, stirring makes it fully dissolve, room
The lower addition benzoic acid of temperature, mixes reaction 5-6h, is slowly added dropwise 1/2 n-hexane, continues to mix instead after completion of dropping
4-5h is answered, is filtered, filter cake is washed 2-3 times with remaining n-hexane, be vacuum dried, obtain emamectin-benzoate；
（2）Diflubenzuron and ethyl acetate are added in reaction vessel, mechanical agitation is well mixed, rise high-temperature to 80-85 DEG C,
Reaction 10-12h is refluxed, is filtered while hot, cool down filtrate, and filtered again, filter cake is washed 2-3 times with dichloromethane, will be filtered
Cake dries 10-12h in 60-65 DEG C of vacuum drying chamber；By dried filter cake and step（1）Product be added to 1/2 third
In ketone, after mixing and stirring, laruyl alcohol sulfosuccinate disodium, 30-40 DEG C of mixing 2-3h is added to be mixed
Liquid；During mixed liquor is added into polyvinyl alcohol and solution equivalent to the deionized water configuration of polyvinyl alcohol weight part 12-15 times,
45-50 DEG C is continued to mix 3-4h, adds xanthans, and 60-65 DEG C is continued to mix 5-6h, centrifugation, deionized water
Washing 2-3 times, vacuum drying；
（3）By step（2）Product, shitosan is added to acetic acid and matches somebody with somebody equivalent to the deionized water of 30-35 times of acetic acid weight portion
In the solution put, after mixing and stirring, the solution of polyethylene glycol and atoleine configuration is added to, in 50-55 DEG C of water-bath
In turned with 2200-2500/the rotating speed constant temperature of min quickly stirs 25-30min, forms white " milky " liquid, leads to nitrogen 20-30min,
The solution of Geniposide and the configuration of remaining acetone is added, 65-70 DEG C is continued to stir 5-6h, is washed with deionized 2-3 times, from
The heart is separated, and 20-24h is dried in 60-65 DEG C of vacuum drying chamber, and the shitosan for obtaining loading emamectin-benzoate delays
Release microballoon；
（4）By step（3）Product, citric acid dibutyl naphthalenesulfonic acid calcium is added to equivalent to step（3）Products weight part 15-
In 20 times of deionized water, ultrasonic disperse 30-40min adds palmitic acid formicester, triethanolamine, with 800-1000 turns/min's
Rotating speed stirs 25-30min, the emamectin-benzoate mite killing suspending agent of the chitin synthesis that are inhibited.
The emamectin-benzoate mite killing suspending agent of described suppression chitin synthesis, it is characterised in that institute
The concentration of the phosphoric acid solution stated is 0.5-0.6mol/L.
Beneficial effects of the present invention are：
The present invention is main acaricide with emamectin-benzoate, and compared to AVM parent, it is to Lepidoptera elder brother
The activity of worm larva is generally improved, and is especially 6 times of AVM to the preventing and treating of acarid；Emamectin-benzoate
Belong to biogenic pesticide, with its unique mechanism of action, be difficult to remain, can be biodegradable, it is safe and environment-friendly the advantages of, meet
Develop the requirement of nuisanceless fruits and vegetables, pollution-free food；Present invention addition diflubenzuron, work is cooperateed with emamectin-benzoate
Can suppress the synthesis of chitin on larva body wall with, diflubenzuron, ovum is unable to normal development, the larva epidermis of hatching lack hardness and
It is dead；The present invention wraps up AVM using shitosan, and obtains sustained-release micro-spheres, not only to chitosan crosslinked using Geniposide
The slow release medicine of energy, extends the service life of medicament, can significantly reduce its resolution ratio in storage, and shitosan energy
Promote medicament to be absorbed by plants rapidly through Stoma of Leaves, further increase miticidal effect；Mite killing suspending agent of the invention can be efficient
Acarid is lured, acarid is effectively killed, with excellent synergistic effect, acaricidal field dosage is reduced, can effectively be subtracted
Few residues of pesticides and the harm to beneficial organism, while reducing cost accounting and mitigating the pollution to environment.
Specific embodiment
The emamectin-benzoate mite killing suspending agent of the suppression chitin synthesis of the present embodiment, it by weighing as follows
The raw material for measuring part is prepared from：8 parts of emamectin benzoate, 150 parts of methyl alcohol, 40 parts of phosphoric acid solution, 250 parts of toluene, acetic acid are different
70 parts of propyl ester, 3 parts of fatty acid monoglyceride, 15 parts of benzoic acid, 200 parts of n-hexane, 5 parts of diflubenzuron, 60 parts of ethyl acetate, dichloro
50 parts of methane, 100 parts of acetone, 2 parts of laruyl alcohol sulfosuccinate disodium, 12 parts of polyvinyl alcohol, 4 parts of xanthans, shitosan 20
Part, 5 parts of acetic acid, 3 parts of polyethylene glycol, 100 parts of atoleine, 5 parts of Geniposide, 1 part of citric acid dibutyl naphthalenesulfonic acid calcium, palmitic acid
3 parts of formicester, 4 parts of triethanolamine, appropriate deionized water.
The emamectin-benzoate mite killing suspending agent of the suppression chitin synthesis of the present embodiment, it by walking as follows
Suddenly it is prepared from：
（1）At room temperature, emamectin benzoate is added in 2/3 methyl alcohol, is stirred to being completely dissolved, be slowly added dropwise phosphoric acid molten
The mixed solution that liquid is configured with remaining methyl alcohol, continues to mix 2h after completion of dropping；1/2 toluene is added, continues to mix
Stirring 2h, is transferred them in ice-water bath, continues to mix 6h, and centrifugation, precipitation is used and pre-cooled to 0 DEG C of residue
Toluene wash 3 times, vacuum drying；Product after vacuum drying is added to equivalent to 4 times of emamectin benzoate weight portion
Deionized water in, stirring dissolve it, add isopropyl acetate, regulation system PH be 8-9, mix 40min after stand
4h, separates organic phase；Fatty acid monoglyceride is added in organic phase, stirring makes it fully dissolve, benzene first is added at room temperature
Acid, mixes reaction 6h, is slowly added dropwise 1/2 n-hexane, continues to mix reaction 5h, filtering, filter cake after completion of dropping
Washed with remaining n-hexane 3 times, be vacuum dried, obtain emamectin-benzoate；
（2）Diflubenzuron and ethyl acetate are added in reaction vessel, mechanical agitation is well mixed, rise high-temperature to 85 DEG C, returned
Stream stirring reaction 12h, is filtered while hot, cools down filtrate, and filters again, and filter cake is washed 3 times with dichloromethane, by filter cake at 65 DEG C
12h is dried in vacuum drying chamber；By dried filter cake and step（1）Product be added in 1/2 acetone, mix equal
After even, laruyl alcohol sulfosuccinate disodium, 40 DEG C of mixing 3h is added to obtain mixed liquor；Mixed liquor is added to poly- second
In enol and the solution configured equivalent to the deionized water of polyvinyl alcohol weight parts 15 times, 50 DEG C are continued to mix 4h, are added
Xanthans, 65 DEG C are continued to mix 6h, and centrifugation, deionized water is washed 3 times, vacuum drying；
（3）By step（2）Product, shitosan is added to acetic acid and configures equivalent to the deionized water of 35 times of acetic acid weight portion
In solution, after mixing and stirring, the solution of polyethylene glycol and atoleine configuration is added to, with 2500 in 55 DEG C of water-baths
Turn/the rotating speed constant temperature of min quickly stirs 30min, forms white " milky " liquid, leads to nitrogen 30min, adds Geniposide and remaining
The solution of acetone configuration, 70 DEG C are continued to stir 6h, are washed with deionized 3 times, centrifugation, are dried in 65 DEG C of vacuum drying chambers
24h, obtains loading the chitosan sustained-release microsphere of emamectin-benzoate；
（4）By step（3）Product, citric acid dibutyl naphthalenesulfonic acid calcium is added to equivalent to step（3）Products weight parts 20
In deionized water again, ultrasonic disperse 40min adds palmitic acid formicester, triethanolamine, is stirred with the rotating speed of 1000 turns/min
30min, the emamectin-benzoate mite killing suspending agent of the chitin synthesis that are inhibited.
Test method：Caught from field and come each 200 of cabbage caterpillar, heart-eating worm, vegetable aphid, planthopper, acarid, every kind of insect
Individually it is placed in plastic tub, the dish leaf 2 of equivalent is put into each plastic tub, by the mite killing suspending agent dilute with water of the present embodiment
500 times, then the mite killing suspending agent after dilution is uniformly sprayed in plastic tub, dish leaf is stirred during sprinkling, make its comprehensively medicine,
Plastic tub bottom retains without liquid, then covers plastic tub with gauze and seals, and then the insect of 24h and 48h is dead after statistics spray
Die rate.
Result of the test：
| The death rate after spray 24h | The death rate after spray 48h | |
| Cabbage caterpillar | 85.6% | 91.2% |
| Heart-eating worm | 86.4% | 93.1% |
| Vegetable aphid | 83.5% | 89.9% |
| Planthopper | 78.2% | 88.2% |
| Acarid | 92.7% | 98.6% |
Claims (3)
1. it is a kind of suppress chitin synthesis emamectin-benzoate mite killing suspending agent, it is characterised in that it is by such as
The raw material of lower weight portion is prepared from：Emamectin benzoate 6-8 parts, methyl alcohol 120-150 parts, phosphoric acid solution 30-40 parts, toluene
200-250 parts, isopropyl acetate 60-70 parts, fatty acid monoglyceride 2-3 parts, benzoic acid 12-15 parts, n-hexane 180-200
Part, diflubenzuron 4-5 parts, ethyl acetate 50-60 parts, dichloromethane 40-50 parts, acetone 80-100 parts, laruyl alcohol sulfosuccinic acid
1-2 parts of ester disodium, polyvinyl alcohol 10-12 parts, xanthans 3-4 parts, shitosan 18-20 parts, acetic acid 4-5 parts, polyethylene glycol 2-3
Part, atoleine 80-100 parts, Geniposide 4-5 parts, 0.5-1 parts of citric acid dibutyl naphthalenesulfonic acid calcium, 2-3 parts of palmitic acid formicester,
Triethanolamine 3-4 parts, appropriate deionized water.
2. according to claims 1 suppression chitin synthesis emamectin-benzoate mite killing suspending agent,
Characterized in that, it is prepared from by following steps：
（1）At room temperature, emamectin benzoate is added in 2/3 methyl alcohol, is stirred to being completely dissolved, be slowly added dropwise phosphoric acid molten
The mixed solution that liquid is configured with remaining methyl alcohol, continues to mix 1-2h after completion of dropping；1/2 toluene is added, continues mixed
Conjunction stirring 1-2h, is transferred them in ice-water bath, continues to mix 5-6h, and centrifugation, precipitation is used and pre-cooled to 0 DEG C
Remaining toluene wash 2-3 time, be vacuum dried；Product after vacuum drying is added to equivalent to emamectin benzoate weight
Measure in the deionized water of 3-4 times of part, stirring dissolves it, add isopropyl acetate, regulation system PH is 8-9, mixes 30-
3-4h is stood after 40min, organic phase is separated；Fatty acid monoglyceride is added in organic phase, stirring makes it fully dissolve, room
The lower addition benzoic acid of temperature, mixes reaction 5-6h, is slowly added dropwise 1/2 n-hexane, continues to mix instead after completion of dropping
4-5h is answered, is filtered, filter cake is washed 2-3 times with remaining n-hexane, be vacuum dried, obtain emamectin-benzoate；
（2）Diflubenzuron and ethyl acetate are added in reaction vessel, mechanical agitation is well mixed, rise high-temperature to 80-85 DEG C,
Reaction 10-12h is refluxed, is filtered while hot, cool down filtrate, and filtered again, filter cake is washed 2-3 times with dichloromethane, will be filtered
Cake dries 10-12h in 60-65 DEG C of vacuum drying chamber；By dried filter cake and step（1）Product be added to 1/2 third
In ketone, after mixing and stirring, laruyl alcohol sulfosuccinate disodium, 30-40 DEG C of mixing 2-3h is added to be mixed
Liquid；During mixed liquor is added into polyvinyl alcohol and solution equivalent to the deionized water configuration of polyvinyl alcohol weight part 12-15 times,
45-50 DEG C is continued to mix 3-4h, adds xanthans, and 60-65 DEG C is continued to mix 5-6h, centrifugation, deionized water
Washing 2-3 times, vacuum drying；
（3）By step（2）Product, shitosan is added to acetic acid and matches somebody with somebody equivalent to the deionized water of 30-35 times of acetic acid weight portion
In the solution put, after mixing and stirring, the solution of polyethylene glycol and atoleine configuration is added to, in 50-55 DEG C of water-bath
In turned with 2200-2500/the rotating speed constant temperature of min quickly stirs 25-30min, forms white " milky " liquid, leads to nitrogen 20-30min,
The solution of Geniposide and the configuration of remaining acetone is added, 65-70 DEG C is continued to stir 5-6h, is washed with deionized 2-3 times, from
The heart is separated, and 20-24h is dried in 60-65 DEG C of vacuum drying chamber, and the shitosan for obtaining loading emamectin-benzoate delays
Release microballoon；
（4）By step（3）Product, citric acid dibutyl naphthalenesulfonic acid calcium is added to equivalent to step（3）Products weight part 15-
In 20 times of deionized water, ultrasonic disperse 30-40min adds palmitic acid formicester, triethanolamine, with 800-1000 turns/min's
Rotating speed stirs 25-30min, the emamectin-benzoate mite killing suspending agent of the chitin synthesis that are inhibited.
3. the emamectin-benzoate mite killing of the suppression chitin synthesis according to claims 1,2 suspends
Agent, it is characterised in that the concentration of described phosphoric acid solution is 0.5-0.6mol/L.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611202582.7A CN106818727A (en) | 2016-12-23 | 2016-12-23 | A kind of emamectin-benzoate mite killing suspending agent for suppressing chitin synthesis and preparation method thereof |
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| CN201611202582.7A CN106818727A (en) | 2016-12-23 | 2016-12-23 | A kind of emamectin-benzoate mite killing suspending agent for suppressing chitin synthesis and preparation method thereof |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101622987A (en) * | 2008-10-24 | 2010-01-13 | 江西正邦化工有限公司 | Emamectin benzoate microcapsule suspending agent and preparation method thereof |
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2016
- 2016-12-23 CN CN201611202582.7A patent/CN106818727A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101622987A (en) * | 2008-10-24 | 2010-01-13 | 江西正邦化工有限公司 | Emamectin benzoate microcapsule suspending agent and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘新等: "《农药安全使用技术》", 30 September 2014, 福建科学技术出版社 * |
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Application publication date: 20170613 |