CN106700749A - Waterborne flame-retardant emulsion - Google Patents
Waterborne flame-retardant emulsion Download PDFInfo
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- CN106700749A CN106700749A CN201610989573.0A CN201610989573A CN106700749A CN 106700749 A CN106700749 A CN 106700749A CN 201610989573 A CN201610989573 A CN 201610989573A CN 106700749 A CN106700749 A CN 106700749A
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
- C09D125/18—Homopolymers or copolymers of aromatic monomers containing elements other than carbon and hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/14—Monomers containing only one unsaturated aliphatic radical containing one ring substituted by heteroatoms or groups containing heteroatoms
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses waterborne flame-retardant emulsion, which comprises an ingredient A and an ingredient B, wherein the ingredient A is prepared through the following steps: (1) uniformly mixing methyl methacrylate, butyl acrylate, water, a surfacetant and diacetone acrylamide, so as to obtain a base solution; (2) uniformly mixing water, the surfacetant, brominated styrene, butyl acrylate, methyl methacrylate and methyl acrylate so as to obtain a pre-emulsion; (3) preparing potassium persulfate into an initiator aqueous solution; and (4) adding 10% pre-emulsion into a base solution, dropwise adding the initiator solution, when the system temperature is increased, dropwise adding the residual pre-emulsion, fully reacting after dropwise adding is finished, regulating the pH value of the system to 7-8 with alkali after reaction is over, then adding a wetting agent and a defoamer, and uniformly mixing all the ingredients so as to obtain the ingredient A; the ingredient B is adipic dihydrazide aqueous solution. A paint film obtained by the emulsion can be crosslinked at a normal temperature, is high in adhesion force, high in coating mechanical performance, achieves the swabbing resistant times of 3000, and achieves the water resistance of 240 hours.
Description
Technical field
The present invention relates to a kind of waterborne flame retardant emulsion.
Background technology
At present, the application field of environment-friendly water-based fire proofing is constantly expanded, and market prospects are bright.In the market is most of aqueous
Add fire retardant such as tetrabromobisphenol A in coating, TDE, deca-BDE etc., its flame retardant effect is to emulsion and fire-retardant
The compatibility of agent, dispersiveness have very big requirement, and water-fast, alkaline-resisting, weatherability is all poor, significantly limit the wide of them
General application.
Till now early in the twentieth century, the whole world starts numerous studies waterborne flame retardant emulsion, and many industrial circles need application
Waterborne flame retardant emulsion.Country's flame-retardant emulsion molecular weight is small at present, and crosslinking degree is not high, and market demands are not reached far.
The content of the invention
It is an object of the invention to provide a kind of waterborne flame retardant emulsion.
Waterborne flame retardant emulsion provided by the present invention includes component A and B component, and the weight ratio of component A and B component is 3-
10:1；
The component A is obtained by following steps：
（1）By 35-55 parts of methyl methacrylate, 50-100 parts of butyl acrylate, 100-170 parts of deionized water, 3-4 parts of surface
Activating agent and 10-20 parts of DAAM are well mixed, and base fluid is obtained；
（2）By 150-200 parts of deionized water, 3-4 parts of surfactant, 180-200 parts of brominated styrene, 30-80 parts of acrylic acid
Butyl ester, 70-90 part methyl methacrylate and 5-10 parts of methyl acrylate are well mixed, and obtain pre-emulsion；
（3）5-10 parts of potassium peroxydisulfate is dissolved in 50-100 parts of deionized water, initiator solution is made into；
（4）Under conditions of 80-90 DEG C of temperature, base fluid, initiator solution and pre-emulsion are mixed is reacted system, is controlled
Reaction temperature processed is at 80-100 DEG C until reaction terminates；Or, under conditions of 80-90 DEG C of temperature, first by pre-emulsion total amount
10% pre-emulsion is added in base fluid, and initiator solution is then added dropwise, and when the temperature of system begins to ramp up, then residue is added dropwise
Pre-emulsion, controlling reaction temperature continues to be protected at 80-100 DEG C at 80-100 DEG C, after completion of dropping during dropwise addition
Temperature reaction is until reaction terminates；Reaction is cooled to less than 50 DEG C after terminating, and the pH value that regulation system is adjusted with alkali is 7-8, then
1-3 parts of wetting agent and 1-2 parts of defoamer are added, component A is obtained final product after being well mixed；
The B component is the adipic dihydrazide aqueous solution.
The waterborne flame retardant emulsion also includes component C, and the weight ratio of component A, B component and component C is 300-1000:
100:2-5。
The component C is thickener.
The concentration of the adipic dihydrazide aqueous solution is 5-9%.
The step（4）In, the time for adding of remaining pre-emulsion is 1-4 hours, and initiator solution will be remaining
Pre-emulsion is all dripped off when being added drop-wise to 10-30 minutes..
The alkali is ammoniacal liquor, sodium carbonate, potassium carbonate, sodium acid carbonate or saleratus.
The present invention is raw materials used to be commercially available prod, and the surfactant is alkylsulfonate, for example, can use Shandong
The neopelex of Jinan Li Chao Chemical Co., Ltd.s production；The wetting agent is water-soluble nonionic surface-active
Agent, for example can be using the wetting agent of the entitled X-450 of Dow Chemical's production；The defoamer is polyethers defoamer,
For example can be using the defoamer of the entitled DF-104 of Dow Chemical's production；The thickener is the poly- ammonia of city's hydrophobically modified
Ester, for example can be using the thickener of the entitled RM-8W of Dow Chemical's production.
Component A of the invention and B component need to be stored individually；When using, by component A: the weight proportion of B component=3-10: 1
Relation, component A and B component is well mixed and forms mixed liquor.The present invention may also include component C i.e. thickener, to increase
Plus viscosity, can be stirred for uniform according to requirements to appropriate component C is added in the mixed liquor of component A and B component；One
As under situation, the weight proportion relation of component A B component and component C is 300-1000:100:2-5.
Step of the present invention（4）In, the foundation of reaction system can take following two modes：One can be by base fluid, draw
Hair agent solution and pre-emulsion are mixed to form reaction system；Two can be first to mix a small amount of pre-emulsion and base fluid, then drip
Plus initiator solution, remaining pre-emulsion is added dropwise again when system temperature begins to ramp up.Preferably with the second way, so more
Beneficial to facilitating controlling reaction temperature.No matter above-mentioned that mode, general control 4-8 hours reaction time of system can make reaction
Fully.Initiator solution requires that the concrete meaning dripped off in 10-30 minutes that remaining pre-emulsion starts dropwise addition is：Trigger
Agent solution first starts that a period of time is added dropwise, and then remaining pre-emulsion starts to be added dropwise, and now initiator solution is also simultaneously in drop
Plus, initiator solution will in remaining pre-emulsion is added drop-wise to the time period of 10-30 minutes whole completion of dropping.
The present invention uses various function monomers, core shell structure molecule side chain IPN is carried out to emulsion particle, by the work that is polymerized
Skill reaches the purpose of invention.Gained paint film is i.e. cross-linking under normal temperature state, has very strong adhesive force, therefore coating to base material
Mechanical performance is greatly improved, and up to 3000 times, water resistance reaches 240h to paint film scrubbing resistance number of times after tested.
Specific embodiment
Technical solution of the present invention is further illustrated below by embodiment, these embodiments are intended merely to represent this hair in detail
Bright technology design and its exploitativeness, is not limiting the scope of the invention, is made using the technology of the present invention design
Equivalence replacement and accommodation still within protection scope of the present invention.
Embodiment 1
Waterborne flame retardant emulsion is made up of component A and B component, and the weight proportion relation of component A and B component is 3:1；Above-mentioned component A
By following steps be obtained：
（1）By 35 parts of methyl methacrylates, 50 parts of butyl acrylates, 100 deionized waters, 3 parts of surfactant sodium dodecyl bases
Benzene sulfonic acid sodium salt and 10 parts of DAAMs are well mixed, and base fluid is obtained；
（2）By 150 parts of deionized waters, 3 parts of surfactant sodium dodecyl base benzene sulfonic acid sodium salts, 180 parts of brominated styrenes, 30 parts of propylene
Acid butyl ester, 70 parts of methyl methacrylates and 5 parts of methyl acrylates are well mixed, and obtain pre-emulsion；
（3）5 parts of potassium peroxydisulfates are dissolved in 50 parts of deionized waters, initiator solution is made into；
（4）Under conditions of 80 DEG C of temperature, during the pre-emulsion of pre-emulsion total amount 10% first added into base fluid, while dropwise addition is drawn
Hair agent solution, when the temperature of system begins to ramp up, then is added dropwise remaining pre-emulsion, and controlling reaction temperature exists during dropwise addition
85 DEG C, the time for adding of remaining pre-emulsion is 3 hours, and initiator solution will be when remaining pre-emulsion be added dropwise 10 minutes
All drip off, continue to carry out insulation reaction at 85 DEG C 2 hours after completion of dropping；Reaction is cooled to less than 50 DEG C after terminating, use
The pH value of ammoniacal liquor regulation regulation system is 8,3 parts of wetting agent X-450 and 1 part of defoamer DF-104 is subsequently adding, after stirring
Obtain final product component A；
It is made into adipic dihydrazide is soluble in water the aqueous solution that mass concentration is 5% and obtains final product B component；
When using, component A and B component are first pressed 3:1 weight proportion relation is mixed, and just be can be used after being well mixed.
Embodiment 2
The waterborne flame retardant emulsion that the present embodiment is provided is made up of component A, B component and component C, component A, B component and component C
Weight proportion relation is 300:100:2；Wherein component A and B component are identical with the component A and B component described in embodiment 1, i.e., originally
Component A and B component in embodiment are prepared as indicated in example 1 and obtain；Component C is RM-8W thickeners；Use
When, component A, B component and component C are first pressed 300:100:2 weight proportion relation is mixed, and can be made after being well mixed
With.
Embodiment 3
Waterborne flame retardant emulsion is made up of component A and B component, and the weight proportion relation of component A and B component is 7:1；Above-mentioned component A
By following steps be obtained：
（1）By 45 parts of methyl methacrylates, 70 parts of butyl acrylates, 150 parts of deionized waters, 4 parts of surfactant sodium dodecyls
Base benzene sulfonic acid sodium salt and 15 parts of DAAMs are well mixed, and base fluid is obtained；
（2）By 170 parts of deionized waters, 4 parts of surfactant sodium dodecyl base benzene sulfonic acid sodium salts, 190 parts of brominated styrenes, 50 parts of propylene
Acid butyl ester, 80 parts of methyl methacrylates and 8 parts of methyl acrylates are well mixed, and obtain pre-emulsion；
（3）8 parts of potassium peroxydisulfates are dissolved in 70 parts of deionized waters, initiator solution is made into；
（4）Under conditions of 90 DEG C of temperature, during the pre-emulsion of pre-emulsion total amount 10% first added into base fluid, while dropwise addition is drawn
Hair agent solution, when the temperature of system begins to ramp up, then is added dropwise remaining pre-emulsion, and controlling reaction temperature exists during dropwise addition
95 DEG C, the time for adding of remaining pre-emulsion is 2 hours, and initiator solution will be added drop-wise to 15 minutes in remaining pre-emulsion
When all drip off, continue to carry out insulation reaction at 95 DEG C 2 hours after completion of dropping；Reaction is cooled to less than 50 DEG C after terminating,
The pH value that regulation system is adjusted with sodium acid carbonate is 7-8, is subsequently adding 2 parts of wetting agent X-450 and 2 parts of defoamer DF-104, is mixed
Component A is obtained final product after closing uniformly；
It is made into adipic dihydrazide is soluble in water the aqueous solution that mass concentration is 6% and obtains final product B component；
When using, component A and B component are first pressed 7:1 weight proportion relation is mixed, and just be can be used after being well mixed.
Embodiment 4
The waterborne flame retardant emulsion that the present embodiment is provided is made up of component A, B component and component C, component A, B component and component C
Weight proportion relation is 300:100:2；Wherein component A and B component are identical with the component A and B component described in embodiment 3, i.e., originally
Component A and B component in embodiment are prepared by the method described in embodiment 3；Component C is RM-8W thickeners.Use
When, component A, B component and component C are first pressed 700:100:3 weight proportion relation is mixed, and can be made after being well mixed
With.
Embodiment 5
Waterborne flame retardant emulsion is made up of component A and B component, and the weight proportion relation of component A and B component is 10:1；Above-mentioned A groups
That divides is obtained by following steps：
（1）By 55 parts of methyl methacrylates, 100 parts of butyl acrylates, 170 parts of deionized waters, 4 parts of surfactant sodium dodecyls
Base benzene sulfonic acid sodium salt and 20 parts of DAAMs are well mixed, and base fluid is obtained；
（2）By 200 parts of deionized waters, 4 parts of surfactant sodium dodecyl base benzene sulfonic acid sodium salts, 200 parts of brominated styrenes, 80 parts of propylene
Acid butyl ester, 90 parts of methyl methacrylates and 10 parts of methyl acrylates are well mixed, and obtain pre-emulsion；
（3）10 parts of potassium peroxydisulfates are dissolved in 100 parts of deionized waters, initiator solution is made into；
（4）Under conditions of 82 DEG C of temperature, during the pre-emulsion of pre-emulsion total amount 10% first added into base fluid, while dropwise addition is drawn
Hair agent solution, when the temperature of system begins to ramp up, then is added dropwise remaining pre-emulsion, and controlling reaction temperature exists during dropwise addition
85 DEG C, the time for adding of remaining pre-emulsion is 1 hour, and initiator solution will be added drop-wise to 30 minutes in remaining pre-emulsion
When all drip off, continue to carry out insulation reaction at 85 DEG C 3 hours after completion of dropping；Reaction is cooled to less than 50 DEG C after terminating,
The pH value that regulation system is adjusted with sodium carbonate is 8, is subsequently adding 3 parts of wetting agent X-450 and 2 parts of defoamer DF-104, and mixing is equal
Component A is obtained final product after even；
It is made into adipic dihydrazide is soluble in water the aqueous solution that mass concentration is 8% and obtains final product B component；
When using, component A and B component are first pressed 7:1 weight proportion relation is mixed, and just be can be used after being well mixed.
Embodiment 6
The waterborne flame retardant emulsion that the present embodiment is provided is made up of component A, B component and component C, component A, B component and component C
Weight proportion relation is 1000:100:5；Wherein component A and B component are identical with the component A and B component described in embodiment 5, i.e.,
Component A and B component in the present embodiment are prepared by the method described in embodiment 5；Component C is RM-8W thickeners.Use
When, component A, B component and component C are first pressed 1000:100:5 weight proportion relation is mixed, and can be made after being well mixed
With.
Embodiment 7
Waterborne flame retardant emulsion is made up of component A and B component, and the weight proportion relation of component A and B component is 3:1；Above-mentioned component A
By following steps be obtained：
（1）By 35 parts of methyl methacrylates, 50 parts of butyl acrylates, 100 deionized waters, 3 parts of surfactant sodium dodecyl bases
Benzene sulfonic acid sodium salt and 10 parts of DAAMs are well mixed, and base fluid is obtained；
（2）By 150 parts of deionized waters, 3 parts of surfactant sodium dodecyl base benzene sulfonic acid sodium salts, 180 parts of brominated styrenes, 30 parts of propylene
Acid butyl ester, 70 parts of methyl methacrylates and 5 parts of methyl acrylates are well mixed, and obtain pre-emulsion；
（3）5 parts of potassium peroxydisulfates are dissolved in 50 parts of deionized waters, initiator solution is made into；
（4）Under conditions of 80 DEG C of temperature, base fluid, pre-emulsion and initiator solution are mixed is reacted system, is controlled
Reaction temperature carries out insulation reaction 5 hours at 85 DEG C, and reaction is cooled to less than 50 DEG C after terminating, and regulation system is adjusted with ammoniacal liquor
PH value is 8, is subsequently adding 3 parts of wetting agent X-450 and 1 part of defoamer DF-104, and component A is obtained final product after stirring；
It is made into adipic dihydrazide is soluble in water the aqueous solution that mass concentration is 5% and obtains final product B component；
When using, component A and B component are first pressed 3:1 weight proportion relation is mixed, and just be can be used after being well mixed.
After testing, its technical indicator of waterborne flame retardant emulsion of the present invention is as shown in the table：
| Sequence number | Detection project | Measured value |
| 1 | Emulsion particle diameter | 60-80nm |
| 2 | Outward appearance | Milky |
| 3 | Solid content, %, >= | 45 |
| 4 | PH | 7.5 |
| 5 | Mechanical stability, 800r/min, 30min | It is not stratified, do not flocculate |
| 6 | Heat-resistant stability, 50 DEG C | It is not stratified, do not flocculate |
| 7 | Freeze-thaw stability, -10 DEG C | It is not stratified, do not flocculate |
| 8 | Adhesive force, cross-hatching, level | 0 |
| 9 | Pencil hardness >= | H |
| 10 | Scrubbing resistance number of times >= | 3000 |
| 11 | Water resistance, 240h | Slightly turn white |
Claims (6)
1. a kind of waterborne flame retardant emulsion, it is characterised in that the emulsion includes the weight ratio of component A and B component, component A and B component
It is 3-10:1；
The component A is obtained by following steps：
（1）By 35-55 parts of methyl methacrylate, 50-100 parts of butyl acrylate, 100-170 parts of deionized water, 3-4 parts of surface
Activating agent and 10-20 parts of DAAM are well mixed, and base fluid is obtained；
（2）By 150-200 parts of deionized water, 3-4 parts of surfactant, 180-200 parts of brominated styrene, 30-80 parts of acrylic acid
Butyl ester, 70-90 part methyl methacrylate and 5-10 parts of methyl acrylate are well mixed, and obtain pre-emulsion；
（3）5-10 parts of potassium peroxydisulfate is dissolved in 50-100 parts of deionized water, initiator solution is made into；
（4）Under conditions of 80-90 DEG C of temperature, base fluid, initiator solution and pre-emulsion are mixed is reacted system, is controlled
Reaction temperature processed is at 80-100 DEG C until reaction terminates；Or, under conditions of 80-90 DEG C of temperature, first by pre-emulsion total amount
10% pre-emulsion is added in base fluid, and initiator solution is then added dropwise, and when the temperature of system begins to ramp up, then residue is added dropwise
Pre-emulsion, controlling reaction temperature continues to be protected at 80-100 DEG C at 80-100 DEG C, after completion of dropping during dropwise addition
Temperature reaction is until reaction terminates；Reaction is cooled to less than 50 DEG C after terminating, and the pH value that regulation system is adjusted with alkali is 7-8, then
1-3 parts of wetting agent and 1-2 parts of defoamer are added, component A is obtained final product after being well mixed；
The B component is the adipic dihydrazide aqueous solution.
2. waterborne flame retardant emulsion according to claim 1, it is characterised in that waterborne flame retardant emulsion also includes component C, A groups
Point, the weight ratio of B component and component C be 300-1000:100:2-5.
3. waterborne flame retardant emulsion according to claim 2, it is characterised in that the component C is thickener.
4. waterborne flame retardant emulsion according to claim 1, it is characterised in that the concentration of the adipic dihydrazide aqueous solution
It is 5-9%.
5. waterborne flame retardant emulsion according to claim 1, it is characterised in that the step（4）In, remaining pre-emulsion
Time for adding be 1-4 hours, initiator solution will all be dripped off when remaining pre-emulsion is added drop-wise to 10-30 minutes.
6. the waterborne flame retardant emulsion according to any claim in claim 1-5, it is characterised in that the alkali be ammoniacal liquor,
Sodium carbonate, potassium carbonate, sodium acid carbonate or saleratus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610989573.0A CN106700749A (en) | 2016-11-10 | 2016-11-10 | Waterborne flame-retardant emulsion |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610989573.0A CN106700749A (en) | 2016-11-10 | 2016-11-10 | Waterborne flame-retardant emulsion |
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| CN106700749A true CN106700749A (en) | 2017-05-24 |
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| CN201610989573.0A Pending CN106700749A (en) | 2016-11-10 | 2016-11-10 | Waterborne flame-retardant emulsion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108624182A (en) * | 2017-11-07 | 2018-10-09 | 株洲飞鹿高新材料技术股份有限公司 | High fire-retardance water-based acrylic resin lotion and high resistant burning coating material |
| CN109731273A (en) * | 2019-01-28 | 2019-05-10 | 西安科技大学 | A kind of green bio resistanceization fireproofing extinguishing materials and preparation method thereof |
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| CN109731273A (en) * | 2019-01-28 | 2019-05-10 | 西安科技大学 | A kind of green bio resistanceization fireproofing extinguishing materials and preparation method thereof |
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Application publication date: 20170524 |