CN107674374A - A kind of Polyether-ether-ketocable cable material and preparation method thereof - Google Patents
A kind of Polyether-ether-ketocable cable material and preparation method thereof Download PDFInfo
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- CN107674374A CN107674374A CN201710968170.2A CN201710968170A CN107674374A CN 107674374 A CN107674374 A CN 107674374A CN 201710968170 A CN201710968170 A CN 201710968170A CN 107674374 A CN107674374 A CN 107674374A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/36—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes condensation products of phenols with aldehydes or ketones
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- C08K2003/265—Calcium, strontium or barium carbonate
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Abstract
A kind of Polyether-ether-ketocable cable material and preparation method thereof, belong to wire cable insulating field of material technology.By polyether-ether-ketone, polyphenylene sulfide, modified crystal whisker of hexa potassium titanate and inorganic nano nucleator make respectively it is dry after mix through high-speed mixer, then by double screw extruder under 250~400 DEG C of temperature conditionss extruding pelletization, obtain Polyether-ether-ketocable cable material granulation.Using CABLE MATERIALS of the present invention, greatly improved compared to common electric wire temperature resistant grade, and resistance to irradiation, mechanical performance and wearability are high, it can be widely applied in the use condition harsh environment such as Aero-Space, automotive electronics, medicine equipment and nuclear power, had broad application prospects in special cable industry.
Description
Technical field
The invention belongs to wire cable insulating field of material technology.
Background technology
Polyether-ether-ketone（PEEK）A kind of special engineering plastics of excellent performance, have high temperature resistant, mechanical performance it is excellent, from
The excellent spies such as lubricity is good, resistant to chemical etching, fire-retardant, peel resistance, radiation property is good, insulating properties is stable, hydrolysis and rub resistance
Property, it is widely used in Aero-Space, electronic apparatus, automobile making, medicine equipment and nuclear industry field.With China
Aero-Space, nuclear industry, petrochemical industry, track traffic and the structure optimization of hygiene medical treatment industry and booming, these fields
Functional requirement to Special Wires and Cables is constantly lifted, such as lightweight, ultra-thin, fire-retardant, low cigarette, nontoxic, high-low temperature resistant, resistance to spoke
According to, it is resistant to chemical etching and wear-resisting etc., high temperature resistant cable in the market can not all meet above-mentioned requirements simultaneously.
The glass transition temperature of PEEK amorphous areas is high（T g= 143℃）, heat resistance is most excellent in thermoplastic resin
, while also there is excellent synthesis mechanics, electric property, it can meet simultaneously by the use of PEEK as novel cable sheath material
State requirement, can as all kinds of high performance cables renewal product be used for Aero-Space, nuclear industry, petrochemical industry, automobile and
The field such as track traffic and medicine equipment.But PEEK melting temperatures are high（T m= 334℃）, and viscosity in the molten state
It is larger, difficulty is brought to its processing and forming, processing characteristics are unsuitable for directly applying to wires and cables industry, it is impossible to directly apply to
The manufacture of electric wire.
Polyphenylene sulfide（PPS）With its excellent high-temperature stability, anti-flammability, chemical resistance and good mechanics and electricity
Learning sexual function also turns into the emphasis of new material research and development, and especially its melt-processable is excellent, by itself and other unmanageable heat
Plastic engineering plastics are blended, and can improve the melt-processable of the latter.PPS is incorporated into PEEK systems, can be notable
Improve PEEK processing fluidity.But PEEK and PPS co-mixing systems only have good compatibility in the molten state, in solid-state
Under the conditions of be in obvious phase-separated state, its macromechanics mechanical performance decreases, and can not meet the need of wires and cables industry
Ask.
The content of the invention
The purpose of the present invention is to overcome deficiency of the prior art, there is provided one kind have excellent machinability and high intensity,
The Polyether-ether-ketocable cable material of high abrasion.
The present invention includes polyether-ether-ketone, polyphenylene sulfide, modified crystal whisker of hexa potassium titanate and inorganic nano nucleator, the modification
Crystal whisker of hexa potassium titanate is modified to crystal whisker of hexa potassium titanate by titanate coupling agent and is prepared.
Potassium titanate crystal whisker is a kind of micro nanometer fiber shape inorganic material, is high-performance composite materials reinforcing fiber material of new generation
Material, it is especially maximum with the practical value of crystal whisker of hexa potassium titanate.Crystal whisker of hexa potassium titanate has excellent chemical stability, excellent resistance to
Mill property, lubricity, high electric insulating quality, excellent mechanics and physical property, it is widely used in strengthening in composite.Through
Cross our in-depth studies to find, add a small amount of crystal whisker of hexa potassium titanate in the PEEK composites that PPS is modified, can suppress
Phase separation of the PEEK and PPS co-mixing systems under solid conditions, so as to while PEEK molding processibilities are improved, avoid machine
The reduction of tool performance, PEEK and PPS composites are made to can be used in the manufacture of high-performance special cable.This method is existing
Had not been reported in patent.
Because PEEK melting temperatures are high, the temperature of extruder head is very high in molding process, and PEEK composites leave
Temperature decrease after head, material internal easily form non-crystalline state.In order to prevent PEEK Special cable materials in complicated use environment
Middle generation stress cracking, we with the addition of a small amount of inorganic nano nucleator in PEEK and PPS co-mixing systems, compound to improve
The crystallinity of material and the ability of anti-stress cracking.
The present invention is blended using PPS and PEEK, to improve PEEK processing fluidity；Add and change in co-mixing system simultaneously
Property crystal whisker of hexa potassium titanate and inorganic nano nucleator, while composite processing is improved, ensure the machinery of composite
Performance is not lost, and the coefficient of friction of composite is greatly reduced.Using CABLE MATERIALS of the present invention, compared to common electric wire
Temperature resistant grade greatly improves, and resistance to irradiation, mechanical performance and wearability are high, can be widely applied to Aero-Space, automotive electronics,
In the use condition harsh environment such as medicine equipment and nuclear power, had broad application prospects in special cable industry.
Further, polyether-ether-ketone of the present invention, polyphenylene sulfide, modified crystal whisker of hexa potassium titanate and inorganic nano nucleator difference
Account for 65%~90%, 5%~30% and the 1%~10% and 0.1%~5% of Polyether-ether-ketocable cable material gross mass.Polyether-ether-ketone is as extraordinary
The main component of CABLE MATERIALS, account for the 65%~90% of gross mass.But polyether-ether-ketone melting temperature is high, melt viscosity is big, and processing is special
Sexual incompatibility directly applies to the manufacture of electric wire, and a small amount of polyphenylene sulfide, which is blended, can significantly improve the processing stream of polyether-ether-ketone
Dynamic property, submember of the polyphenylene sulfide as CABLE MATERIALS, accounts for the 5%~30% of gross mass.But polyether-ether-ketone and polyphenylene sulfide exist
It is in obvious phase-separated state under solid conditions, the mechanics mechanical performance of intermingling material can not meet the need of wires and cables industry
Ask.Found by our in-depth studies, it is brilliant that a small amount of potassium hexatitanate is added in polyether-ether-ketone and polyphenyl thioether composite material
Must, phase separation of the co-mixing system under solid conditions can be suppressed, the manufacture of high-performance special cable can be used for.Six titaniums
Sour potassium whisker accounts for the 1%~10% of gross mass, can not suppress the phase separation of polyether-ether-ketone and polyphenylene sulfide less than 1%, more than 10% 6
Potassium titanate crystal whisker can reunite in matrices of composite material, make the performance of composite reduce.Because polyether-ether-ketone melts temperature
Degree is high, and the temperature of extruder head is very high in molding process, and polyether-ether-ketone composite material leaves temperature decrease after head, material
It is internal easily to form non-crystalline state, stress cracking easily occurs in complicated use environment.A small amount of inorganic nano nucleator is added,
Polyether-ether-ketone and polyphenyl thioether composite material can be made during temperature decrease, rapidly partially crystallizable, improve composite wood
The crystallinity of material and the ability of anti-stress cracking.Inorganic nano nucleator accounts for the 0.1%~5% of gross mass, can not be produced less than 0.1%
Raw enough nucleus, easily reunite in matrices of composite material more than 5%, influence the performance of composite.
The preparation method of the modified crystal whisker of hexa potassium titanate is：First titanate coupling agent is mixed with water and ethanol,
Mixed solvent is obtained, then by crystal whisker of hexa potassium titanate and mixed solvent after ultrasonic disperse, evaporates mixed solvent, obtains modified six titaniums
Sour potassium whisker.There is the hydroxyl of many on crystal whisker of hexa potassium titanate surface, and surface is hydrophilic and oleophobic property, is directly appended in composite
It is difficult to be uniformly dispersed, it is necessary to carry out surface modification to crystal whisker of hexa potassium titanate, in its surface modification lipophilic group, have its surface
There is a lipophilic-hydrophobic property, improve scattered, wetting of the crystal whisker of hexa potassium titanate in organic matrix and the caking property with organic matrix resin.
The titanate coupling agent is pyrophosphoric acid type alcoxyl base class titanate esters, a diameter of the 0.2~1.5 of crystal whisker of hexa potassium titanate
μm, length is 10~50 μm.The method that the surface of crystal whisker of hexa potassium titanate is modified at present is mainly modified using coupling agent,
But whisker structure is more regular, surface is smooth, surface more chemical inertness, and it is anti-chemistry directly can not to occur with most coupling agents
Should.And pyrophosphoric acid type alcoxyl base class titanate esters are a kind of preferably coupling agents, surface directly can be carried out to crystal whisker of hexa potassium titanate
It is modified.
Crystal whisker of hexa potassium titanate size is tiny, easily reunites and puts up a bridge, and then influences point of the whisker in organic matrix resin
Dissipate property.Learnt by many experiments, using the diameter of whisker at 0.2~1.5 μm, length is in 10~50 μ ms, in solid-liquid
In phase dispersion process, the Zeta potential on whisker surface and between space spacing it is relatively mild, warm-up movement in dispersion liquid and
It is difficult to draw close and reunite in Brownian motion process.And do not occur after with coupling agent surface modification, in drying process secondary yet
Particle and three times particle agglomeration.
The mixing quality ratio of the titanate coupling agent and crystal whisker of hexa potassium titanate is 1~3: 100.By repeatedly substantial amounts of real
Display is tested, when the mixing quality of titanate coupling agent and crystal whisker of hexa potassium titanate ratio is more than 3%, titanate coupling agent is excessive；And
When in the range of this, titanate coupling agent can be reacted completely, and appropriate oleophylic functional group is introduced on crystal whisker of hexa potassium titanate surface, is kept away
Exempt from crystal whisker of hexa potassium titanate reunion, and have good dispersiveness in organic matrix；When titanate coupling agent and crystal whisker of hexa potassium titanate
Mixing quality ratio when being less than 1%, crystal whisker of hexa potassium titanate surface is modified incomplete, and whisker is reunited, it is impossible in matrix resin
Disperse well.
Inorganic nano nucleator of the present invention is nano imvite, nanometer galapectite, nano-attapulgite, nanometer two
In silica or nano-calcium carbonate at least any one.Because polyether-ether-ketone melting temperature is high, extruded in molding process
The temperature of head is very high, and polyether-ether-ketone composite material leaves temperature decrease after head, and material internal easily forms non-crystalline state, easily
Stress cracking occurs in complicated use environment.Nano imvite, nanometer galapectite, nano-attapulgite, nano silicon
Or nano-calcium carbonate is the business inorganic nano material that conventional low price is easy to get, generally makes an addition in matrix resin and be used to improve again
The mechanical property of condensation material, we only add a small amount of inorganic nano material as nucleator, can make polyether-ether-ketone and polyphenyl
Thioether composite is during temperature decrease, and rapidly partially crystallizable, the crystallinity and resistance to stress for improving composite are opened
The ability split.
The present invention is another object is that propose the preparation method of above Polyether-ether-ketocable cable material.
Preparation method of the present invention is：By polyether-ether-ketone, polyphenylene sulfide, modified crystal whisker of hexa potassium titanate and inorganic nano nucleator
Mixed after system is dry respectively through high-speed mixer, then extruded and made under 250~400 DEG C of temperature conditionss by double screw extruder
Grain, obtain Polyether-ether-ketocable cable material granulation.
The polyether-ether-ketone, polyphenylene sulfide, modified crystal whisker of hexa potassium titanate and nucleator account for respectively the quality that always feeds intake 65% ~
90%th, 5%~30% and 1%~10% and 0.1%~5%.
PEEK is a kind of semi-crystalline state aromatic thermoplastic engineering plastics in above-mentioned technical proposal, in the art based on
Material, it can guarantee that the basic performance of Special cable material product.
PPS is a kind of excellent armaticity thermoplastic engineering plastic of melt-processable, and a small amount of PPS and PEEK are total to
It is mixed, the problem of PEEK molten condition viscosity is larger can be improved, solve the problems, such as pure PEEK materials processing and forming difficulty.
Crystal whisker of hexa potassium titanate is a kind of other one dimension fibre shape inorganic material of micro/nano level, and size is trickle, can extruded
It is homogeneously dispersed in mixed process in PEEK and PPS composites, suppresses PEEK and PPS co-mixing systems under solid conditions
It is separated, is that PEEK and PPS composites can be used in high-performance special so as to avoid the reduction of composite machinery performance
The manufacture of cable.
Inorganic nano nucleator is inorganic nano material, PEEK and PPS composites can be made to crystallize in a short time, kept away
Exempt from after composite leaves extruder head, due to temperature decrease, material internal forms non-crystalline state, so as to improve composite
Crystallinity and anti-stress cracking ability.
Compared with prior art, the present invention has the following advantages that and effect：
1. the present invention is blended using PPS and PEEK, PPS is incorporated into PEEK systems, PEEK processing flowing can be significantly improved
Property.Crystal whisker of hexa potassium titanate is one-dimensional material, and size is trickle, can be flowed everywhere with PEEK compound resins during extrusion mixing
It can arrive, therefore fillibility, good fluidity, can preferably it be scattered in PEEK and PPS composite, especially PEEK and PPS
Interface on.The growth course of crystal whisker of hexa potassium titanate determines that its molecule is flawless, and the bending strength of whisker in itself is several
Level off to theoretical maximum, thus the crystal whisker of hexa potassium titanate on the interface in PEEK and PPS can greatly improve only with
The mechanics mechanical performance of PEEK and PPS blended compound materials.
Crystal whisker of hexa potassium titanate of the present invention carries out surface modification using titanate coupling agent, in crystal whisker of hexa potassium titanate
Surface introduces alkoxy, it is possible to increase dispersiveness of the whisker in resin matrix, it is compatible with PEEK and PPS interface to solve whisker
Problem, increase the combination of whisker and resin matrix, the phase separation that can not only improve PPS blendings PEEK is asked questions, while also can
Improve the mechanics mechanical performance and wearability of composite.
2. the present invention is improving PEEK products using the scheme for adding inorganic nano nucleator on a small quantity in the composite
While processability, PEEK crystallinity is improved, composite is quickly extrusion-molded into CABLE MATERIALS, and with higher
Mechanical strength and wearability.
3. the present invention is remaining PEEK materials high-low temperature resistants itself, fire-retardant, chemical resistance, oil resistivity, resistance to stripping
On the basis of the excellent properties such as property, the extrusion processability of PEEK materials is improved, is adapted to the application of wires and cables industry；And
Improve the mechanics mechanical performance and wearability of PEEK composites.
Using CABLE MATERIALS of the present invention, greatly improved compared to common electric wire temperature resistant grade, and resistance to irradiation, machinery
Performance and wearability are high, can be widely applied to the harsh ring of the use conditions such as Aero-Space, automotive electronics, medicine equipment and nuclear power
In border, had broad application prospects in special cable industry.
Embodiment
The present invention is described in detail with reference to preferred embodiment, so that advantages and features of the invention can be more
It is easy to be readily appreciated by one skilled in the art.
First, the preparation of modified crystal whisker of hexa potassium titanate：
By 1~3g titanate coupling agents --- pyrophosphoric acid type monoalkoxy class titanate esters TMC-114 or KR-38S are added to 10 mL
In water and 20 mL alcohol mixed solvents.After stirring 30 min, by 100g is a diameter of 0.2~1.5 μm, length is 10~50 μm
Crystal whisker of hexa potassium titanate be added in above titanate coupling agent solution, the h of ultrasonic disperse 1, then rotary evaporation remove solvent second
Alcohol and water, obtain the crystal whisker of hexa potassium titanate of 100 g surfaces modification.
2nd, the preparation of Polyether-ether-ketocable cable material：
Example 1：
PEEK, PPS, modified crystal whisker of hexa potassium titanate and nanometer galapectite are placed in convection oven respectively, done under the conditions of 120 DEG C
Dry 2 h.
The PEEK of 75kg dryings, the modification crystal whisker of hexa potassium titanate that the PPS that 18kg is dried, 6kg are dried are weighed respectively, and 1kg is done
Dry nanometer galapectite.
It each dispensing will be mixed above using high-speed stirring mixer, and obtain compound.
Compound is fully melted under 250~400 DEG C of technological temperatures by double screw extruder again, mix after extruded stock
Bar, cooling granulation, Polyether-ether-ketocable cable material is produced, labeled as sample 1.
Example 2：
PEEK, PPS, modified crystal whisker of hexa potassium titanate, nanometer galapectite, nano-calcium carbonate are placed in convection oven respectively, in 120
2 h are dried under the conditions of DEG C.
The PEEK of 80kg dryings, the modification crystal whisker of hexa potassium titanate that the PPS that 14kg is dried, 4kg are dried are weighed respectively, and 1kg is done
The nano-calcium carbonate that dry nanometer galapectite and 1kg are dried.
Dispensing is mixed using high-speed stirring mixer, obtains compound.
Compound is fully melted under 250~400 DEG C of technological temperatures by double screw extruder again, mix after extruded stock
Bar, cooling granulation, Polyether-ether-ketocable cable material is produced, labeled as sample 2.
Example 3：
PEEK, PPS, modified crystal whisker of hexa potassium titanate, nano-attapulgite are placed in convection oven respectively, under the conditions of 120 DEG C
Dry 2 h.
The PEEK of 85kg dryings, the modification crystal whisker of hexa potassium titanate that the PPS that 11kg is dried, 3kg are dried are weighed respectively, and 1kg is done
Dry nano-attapulgite.
Dispensing is mixed using high-speed stirring mixer, obtains compound.
Compound is fully melted under 250~400 DEG C of technological temperatures by double screw extruder again, mix after extruded stock
Bar, cooling granulation, Polyether-ether-ketocable cable material is produced, labeled as sample 3.
3rd, stretching and bend test contrast：
Using pure PEEK as contrast material, by the CABLE MATERIALS sample obtained by pure PEEK, embodiment 1,2 and 3 respectively according to GB/T
1040-2006 and GB/T 9341-2008 prepare the standard specimen of tension test and bend test, are respectively labeled as control sample
With sample 1, sample 2, sample 3.
Before test, by sample be placed in temperature be 23 ± 2 DEG C, 48 h in the environment of relative humidity is 50%, then respectively will afterwards
Each sample is stretched and bend test, and gained mechanical property is as shown in table 1.From table 1, two performances of sample 1,2 and 3
Index substantially exceeds pure PEEK.
The tensile strength of the various sample of table 1 and the result of the test of bending strength
| Mechanical strength | Unit | Control sample | Sample 1 | Sample 2 | Sample 3 |
| Tensile strength | MPa | 75 | 92 | 98 | 103 |
| Bending strength | MPa | 161 | 163 | 169 | 171 |
Therefore, the PEEK composite cable materials that prepared by present invention process not only have good processability, also have higher mechanics
Mechanical strength.
Claims (9)
1. a kind of Polyether-ether-ketocable cable material, it is characterised in that including polyether-ether-ketone, polyphenylene sulfide, modified crystal whisker of hexa potassium titanate and nothing
Machine nano-nucleating agent, the modified crystal whisker of hexa potassium titanate are modified to crystal whisker of hexa potassium titanate by titanate coupling agent and are prepared.
2. Polyether-ether-ketocable cable material according to claim 1, it is characterised in that the polyether-ether-ketone, polyphenylene sulfide, modified six
Potassium titanate crystal whisker and inorganic nano nucleator account for respectively Polyether-ether-ketocable cable material gross mass 65%~90%, 5%~30% and 1%~
10% and 0.1%~5%.
3. Polyether-ether-ketocable cable material according to claim 1, it is characterised in that the inorganic nano nucleator is that nanometer illiteracy is de-
In soil, nanometer galapectite, nano-attapulgite, nano silicon or nano-calcium carbonate at least any one.
4. the preparation method of Polyether-ether-ketocable cable material as claimed in claim 1, it is characterised in that：By polyether-ether-ketone, polyphenylene sulfide,
It is modified crystal whisker of hexa potassium titanate and inorganic nano nucleator is made after doing and mixed through high-speed mixer respectively, then passes through twin-screw extrusion
Machine extruding pelletization under 250~400 DEG C of temperature conditionss, obtain Polyether-ether-ketocable cable material granulation.
5. preparation method according to claim 4, it is characterised in that：The polyether-ether-ketone, polyphenylene sulfide, modified six metatitanic acids
Potassium whisker and nucleator account for 65% ~ 90%, 5%~30% and the 1%~10% and 0.1%~5% of the quality that always feeds intake respectively.
6. preparation method according to claim 4, it is characterised in that：The preparation method of the modified crystal whisker of hexa potassium titanate
It is：First titanate coupling agent is mixed with water and ethanol, obtains mixed solvent, then by crystal whisker of hexa potassium titanate and mixed solvent
After ultrasonic disperse, mixed solvent is evaporated, obtains being modified crystal whisker of hexa potassium titanate.
7. preparation method according to claim 6, it is characterised in that：The titanate coupling agent is pyrophosphoric acid type list alcoxyl
Base class titanate esters.
8. preparation method according to claim 6, it is characterised in that：A diameter of the 0.2~1.5 of the crystal whisker of hexa potassium titanate
μm, length is 10~50 μm.
9. according to the preparation method described in claim 6 or 7 or 8, it is characterised in that：The titanate coupling agent and potassium hexatitanate
The mixing quality ratio of whisker is 1~3: 100.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677967A (en) * | 2022-09-06 | 2023-02-03 | 山东一诺威聚氨酯股份有限公司 | Caster wear-resistant weather-resistant TPU material and preparation method thereof |
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| CN102329477A (en) * | 2011-06-24 | 2012-01-25 | 深圳市科聚新材料有限公司 | Modification-enhanced polyether ether ketone material and preparation method thereof |
| CN103450631A (en) * | 2013-09-09 | 2013-12-18 | 苏州德尔泰高聚物有限公司 | Polyether-ether-ketone cable material and preparation method thereof |
| CN106674885A (en) * | 2016-12-23 | 2017-05-17 | 张家港大塚化学有限公司 | Method for preparing potassium hexatitanate crystal whisker reinforced composite material |
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Application publication date: 20180209 |