CN107641845A - Polyester-base nano hydridization is fire-retardant/preparation method of antibiotic multifunction fiber and products thereof and application - Google Patents
Polyester-base nano hydridization is fire-retardant/preparation method of antibiotic multifunction fiber and products thereof and application Download PDFInfo
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- CN107641845A CN107641845A CN201711100316.8A CN201711100316A CN107641845A CN 107641845 A CN107641845 A CN 107641845A CN 201711100316 A CN201711100316 A CN 201711100316A CN 107641845 A CN107641845 A CN 107641845A
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Abstract
The present invention relates to polyester-base nano hydridization it is fire-retardant/preparation method of antibiotic multifunction fiber and products thereof and application, using a variety of additives of different nature such as montmorillonite, inorganic nano fire retardant, hydrotalcite and glass fibre, inorganic nano antiseptic, polyester master particle is carried out poly modified, it is blended in high-speed mixer, and extruding pelletization is carried out using double screw extruder, obtain object multiple elements design modified poly ester master batch, then spinning.The present invention realizes the high dispersive of inorganic nanometer functional component, breaches the high key technology for carrying content nano-particle polyester fiber.Product of the present invention, there is good spinnability, antibiotic property and anti-flammability.Fire retardant is halogen-free flame retardants, using with it is safe and non-toxic in combustion process;Antiseptic is serial to carry silver, has long-acting slow-release, and not easy to change, is a kind of green material.The polyester-base nano hydridization of the present invention is fire-retardant/and antibiotic multifunction fiber has good spinnability, antibiotic property and anti-flammability.
Description
Technical field
The present invention relates to a kind of polyester-base nano hydridization it is fire-retardant/preparation method of antibiotic multifunction fiber and products thereof and should
With belonging to organic/inorganic composite modification material technical field.
Background technology
In the modern life, exclude outside natural disaster and war, main disaster precisely due to people's carelessness and caused by fire.
It is fiery caused by textile according to counting and textile is due to the main material that the structural property of itself is initiation fire
Calamity is up to more than 50%.Polyester, including PET, PLA, PBT etc., its fiber is the conjunction that yield is maximum, purposes is most wide in the world at present
Into fiber, more than the 80% of China's chemical fibre total amount is accounted for, very important status is occupied in textile of chemical fibre industry restructuring.It is poly-
Ester has many advantages, such as that its textile application is extensive, it has also become the kind that purposes is most wide, consumption is maximum, therefore its is flame-retarded
More cause worldwide extensive concern.Therefore it is imperative flame retardant treatment to be carried out to a part of textile.
The research of fire-retardant polyester fibre is always a focus of polyester research.From the 1960s so far, the world hinders
Combustion agent market is flourished, and BACN kind emerges in an endless stream, but mainly halogen system, the phosphorus system fire-retardant for PET.Resistance at present
Retardant polyester and fiber mainly use addition type or reactive flame retardant, but this frequently results in and deteriorates some performances of material, causes
Some environmental problems, with this conventional method come assign the anti-flammability of polyester and fiber be with sacrifice or lower material some are precious
Your attribute is cost.
The polymer/inorganic thing nano composite material that late 1980s and the beginning of the nineties rise opens fire-retardant high score
The new way of sub- material, it is possible to reduce the dosage of conventional flame retardants, and can keep or even improve the original performance of polyester, drop
Low amount of flame-retardant agent, also make polyester that there is resistance to molten drop effect.It is fire retardant applied to macromolecule by the inorganic combustion inhibitor of fine
An emerging popular research field in field.It can be both added separately in polyester, also can be with traditional fire-retardant material
Expect compounding use.After especially adding nano-complex, the heat endurance and fire resistance of material improve a lot, in addition, by
In addition than traditional inorganic material much less, thus mechanics on material and physical property influence it is smaller, so being a kind of
The novel flame redundant material of great application prospect, the revolution of flame-retarded technology is described as by foreign countries.
The new development trend of the current anti-flaming function fiber of exploitation of durable efficient, complex function fire resistance fibre, widens original
There is the application field of single fire resistance fibre, meet the multiple demand in market, increase value-added content of product, strengthen the market of product
Competitiveness.
The present invention is led by market demand, respectively with the antibacterial with very big market prospects and flame retardant polyester functional fibre
For core, multi-functional polyester staple fiber is developed.
The content of the invention
The present invention is directed to deficiencies of the prior art, present invention aims at:It is miscellaneous to provide a kind of polyester-base nano
Change the preparation method of fire-retardant/antibiotic multifunction fiber.
Another object of the present invention is:Product prepared by a kind of above method is provided.
Another object of the present invention is:A kind of application of the said goods is provided.
The object of the invention is realized by following proposal:A kind of polyester-base nano hydridization is fire-retardant/system of antibiotic multifunction fiber
Preparation Method, including:
(1)Dried polyester master particle, including montmorillonite, inorganic nano fire retardant, the composite flame-proof of hydrotalcite and glass fibre
Agent, inorganic nano antiseptic, coupling agent, light, oxygen stabilizer, including the lubricant of stearic acid and atoleine, by following quality
Add in high-speed mixer and be well mixed:
1 750 grams of polyester master particle
24 ~ 10 grams of montmorillonites
3 13 ~ 40 grams of inorganic nano fire retardants
4 1.5-10 grams of hydrotalcites
54 ~ 15 grams of glass fibres
6 7.5 ~ 37.5 grams of inorganic nano antiseptics
7 2.12 ~ 3.18 grams of coupling agents
8 0.5 gram of light stabilizers
92 grams of antioxidants
10 2 grams of stearic acid ~ 3 grams
11 6 grams of atoleines ~ 8 grams;
(2)Under the conditions of 30-180 DEG C, stir and evenly mix, then under the conditions of 240-300 DEG C, put into double screw extruder, melt
Melt blending extrusion granulation, obtain fire-retardant/antibiotic multifunction complex polyester master batch so that retardant load level is the 3- of polyester
10wt%, inorganic nano antiseptic addition are the 1-5wt% of polyester, wherein, twin screw extrusion process condition is:Set an area extremely
The design temperature of No.12 District is between 160-220 DEG C of scope, 200-220 DEG C of die temperature, screw speed 100-
200rpm, feeding frequency are 6-12Hz, and multiple elements design modified polyester fiber master batch is prepared by extruding and pelletizing process;
(3)Above-mentioned polyester composite master batch is dried, is subsequently cooled to 40-90 DEG C, adds dispersant, obtains spinning original
Material, spinning is carried out, drawing-off processing, produces fire-retardant/antibiotic multifunction composite polyester fiber, the wherein addition of dispersant is spinning
The 0.1-2wt% of raw material.
On the basis of such scheme, step(1)The inorganic nano fire retardant be particle diameter less than 200 nanometers aluminum oxide,
One or more in magnesia, silica, red phosphorus, expanded graphite;Described glass fibre is the glass that draw ratio is more than 10
Fiber.
In the present invention, using montmorillonite, inorganic nano fire retardant, hydrotalcite and glass fibre, inorganic nano antiseptic
Etc. a variety of additives of different nature, polyester master particle is carried out it is poly modified, and be aided with light stabilizer, antioxidant, lubricant,
Coupling agent etc., is blended in high mixer, and carries out extruding pelletization using double screw extruder, obtains object multiple elements design
Modified poly ester master batch, then spinning.The present invention realizes the high dispersive of inorganic nanometer functional component, breaches high load content nanometer
The key technology of particle polyester fiber, polyester-base nano hydridization of the invention is fire-retardant/and antibiotic multifunction fiber has and well may be used
The property spun, antibiotic property and anti-flammability.
Step(1)In, inorganic nano antiseptic is one kind or several in silver-loaded zirconium phosphate, the silver-colored glass of load, load silver silicate
Kind.
Step(1)In, described coupling agent is titanate coupling agent or silane coupler.
The step(3)Middle dry polyester composite master batch method is:Forced air drying 1-5h at 80-140 DEG C, then will
It is put into 110-170 DEG C of dry 12-60h in vacuum drying chamber.
The step(3)Middle dispersant is one or both of pentaerythritol stearate, ethylene bis stearic acid amide.
The step(3)Middle spinning technology parameter is:Composite spinning machine carries out spinning, 240-300 DEG C of spinning temperature, spinning
Winding speed is 600-3000m/min.
The step(3)Middle drawing-off machined parameters are 1-3.5 times of drafting multiple, 50-90 DEG C of temperature of heat plate, hot plate temperature
120-200℃。
The present invention provide a kind of polyester-base nano hydridization it is fire-retardant/antibiotic multifunction fiber, it is characterised in that according to above-mentioned
One methods described is prepared.
The present invention provides a kind of application of polyester-base nano hydridization multifunctional fibre in fire-retardant/antibacterial.
The present invention is advantageous in that:The high dispersive of inorganic nanometer functional component is realized, breaches high load content nanometer
The key technology of particle polyester fiber, polyester-base nano hydridization of the invention is fire-retardant/antibiotic multifunction fiber, fire retardant is Halogen
Fire retardant, using with it is safe and non-toxic in combustion process, the fiber is a kind of green material;Antiseptic has to carry silver series
There is long-acting slow-release, and it is not easy to change, there is good spinnability, antibiotic property and anti-flammability.
Embodiment
Below by embodiment, the present invention is further elaborated, and its purpose, which is only that, is best understood from present disclosure.
Therefore, the cited case is not intended to limit protection scope of the present invention.
Embodiment 1
(1)By 750g polyester master particles, 4g micro-nano montmorillonite powders, particle diameter is less than 200 nanometers of 40 grams of magnesium oxide powder, neatly
1.5 grams of stone, 15 g glass fibres, 15 grams of silver-loaded zirconium phosphate, 2.12g silane couplers KH560,0.5g light stabilizer, 2g antioxygens
Agent, 2.5g stearic acid, 7g atoleines add high mixer, with standby after 700rpm rotating speed mixing 6min.
By in above-mentioned well mixed raw material input double screw extruder, the design temperature in the area of twin-screw one to No.12 District is
170-220 DEG C, die head sets 210 DEG C, screw speed 190rpm, and feeding frequency is 9Hz.
(2)By obtained fire-retardant/antibiotic multifunction polyester master particle at 110 DEG C forced air drying 2 hours, then put
Enter in vacuum drying chamber 130 DEG C of dryings 48 hours, be cooled to 60 DEG C, add ethylene bis stearic acid amide and obtain spinning material, institute
The addition for stating ethylene bis stearic acid amide is the 0.4wt% of spinning material, and spinning material is added in melt spinning machine and spun
Silk, 265 DEG C of spinning temperature, spinning winding speed are 1000m/min, obtained nascent fire resistance fibre, on Barmag drafting machines
First break draft processing is carried out, obtains fire-retardant/antibiotic multifunction polyester fiber, wherein 2.7 times of drafting multiple, 60 DEG C of temperature of heat plate, heat
140 DEG C of plate temperature.
Using fire-retardant made from the method/antibiotic multifunction polyester fiber filament number:1.5 ~ 2.5dtex, fracture strength
>=3.5CN/dtex, elongation at break >=15%, line density deviation ratio ± 6.0;By obtained fiber woven into fabric, root GB/
T5454-1997《Textile combustion performance test oxygen index method》Measure the LOI of the fire-retardant/antibiotic multifunction Polyester Fibers
For 29%, Escherichia coli antibiotic rate is 95%.
Embodiment 2
(1)By 750g polyester master particles, 10g micro-nano montmorillonite powders, particle diameter is less than 200 nanometers of 5 grams of magnesium oxide powder, oxidation
10 grams of aluminium, 5 grams of hydrotalcite, 10 g glass fibres carry silver-colored 30 grams of glass, 2.36g silane couplers KH570,0.5g light stabilizer,
2g antioxidant, 2g stearic acid, 6g atoleines add high mixer, with standby after 700rpm rotating speed mixing 5min.
By in above-mentioned well mixed raw material input double screw extruder, the design temperature in the area of twin-screw one to No.12 District is
180-220 DEG C, die head sets 215 DEG C, screw speed 180rpm, and feeding frequency is 8Hz.
(2)By obtained fire-retardant/antibiotic multifunction polyester master particle at 110 DEG C forced air drying 2 hours, then put
Enter in vacuum drying chamber 135 DEG C of dryings 48 hours, be cooled to 50 DEG C, add pentaerythritol stearate and obtain spinning material, institute
The addition for stating pentaerythritol stearate is the 0.6wt% of spinning material, and spinning material is added in melt spinning machine and spun
Silk, 270 DEG C of spinning temperature, spinning winding speed are 800m/min, obtained nascent fire resistance fibre, on Barmag drafting machines
First break draft processing is carried out, obtains fire-retardant/antibiotic multifunction polyester fiber, wherein 3.0 times of drafting multiple, 70 DEG C of temperature of heat plate, heat
150 DEG C of plate temperature.
Using fire-retardant made from the method/antibiotic multifunction polyester fiber filament number:1 ~ 3dtex, fracture strength >=
3.0CN/dtex, elongation at break >=15%, line density deviation ratio ± 5.0;By obtained fiber woven into fabric, according to GB/
T5454-1997《Textile combustion performance test oxygen index method》The LOI for measuring the fire-retardant Regenerated Polyester Fibres material is 30%,
The antibiotic rate of Escherichia coli is 99%.
Embodiment 3
(1)By 750g polyester master particles, 6g micro-nano montmorillonite powders, particle diameter is less than 200 nanometers of 25 grams of expanded graphite, hydrotalcite
10 grams, 4g glass fibres carry silver-colored 7.5 grams of glass, 3.18g Silane coupling agent KH550s, 0.5g light stabilizers, 2g antioxidant, and 3g is hard
Resin acid, 8g atoleines add high mixer, with standby after 800rpm rotating speed mixing 6min.
By in above-mentioned well mixed raw material input double screw extruder, the design temperature in the area of twin-screw one to No.12 District is
190-220 DEG C, die head sets 210 DEG C, screw speed 180rpm, and feeding frequency is 8Hz.
(2)By obtained fire-retardant/antibiotic multifunction polyester master particle at 100 DEG C forced air drying 2 hours, then put
Enter in vacuum drying chamber 125 DEG C of dryings 48 hours, be cooled to 40 DEG C, add ethylene bis stearic acid amide and obtain spinning material, institute
The addition for stating ethylene bis stearic acid amide is the 0.8wt% of spinning material, and spinning material is added in melt spinning machine and spun
Silk, 265 DEG C of spinning temperature, spinning winding speed are 800m/min, obtained nascent fire resistance fibre, on Barmag drafting machines
First break draft processing is carried out, obtains fire-retardant/antibiotic multifunction polyester fiber, wherein 3 times of drafting multiple, 60 DEG C of temperature of heat plate, hot plate
140 DEG C of temperature.
Using fire-retardant made from the method/antibiotic multifunction polyester fiber filament number:1.5 ~ 3.0dtex, fracture strength
>=3.0CN/dtex, elongation at break >=20%, line density deviation ratio ± 8.0;By obtained fiber woven into fabric, according to GB/
T5454-1997《Textile combustion performance test oxygen index method》Measure the LOI of the fire-retardant/antibiotic multifunction Polyester Fibers
For 29%, the antibiotic rate of Escherichia coli is 90%.
Embodiment 4
By 750g polyester master particles, 7g micro-nano montmorillonite powders, particle diameter is less than 200 nanometers of 20 grams of expanded graphite, 20 grams of red phosphorus,
8 grams of hydrotalcite, 6g glass fibres carry silver-colored 37.5 grams of silicate, 2.88g silane couplers KH560,0.5g light stabilizer, and 2g resists
Oxygen agent, 3g stearic acid, 7g atoleines add high mixer, with standby after 750rpm rotating speed mixing 5min.
By in above-mentioned well mixed raw material input double screw extruder, the design temperature in the area of twin-screw one to No.12 District is
185-220 DEG C, die head sets 215 DEG C, screw speed 180rpm, and feeding frequency is 8Hz.
(2)By obtained fire-retardant/antibiotic multifunction polyester master particle at 105 DEG C forced air drying 3 hours, then put
Enter in vacuum drying chamber 130 DEG C of dryings 48 hours, be cooled to 50 DEG C, add ethylene bis stearic acid amide and obtain spinning material, institute
The addition for stating ethylene bis stearic acid amide is the 0.5wt% of spinning material, and spinning material is added in melt spinning machine and spun
Silk, 278 DEG C of spinning temperature, spinning winding speed are 1000m/min, obtained nascent fire resistance fibre, on Barmag drafting machines
First break draft processing is carried out, obtains fire-retardant/antibiotic multifunction polyester fiber, wherein 3 times of drafting multiple, 70 DEG C of temperature of heat plate, hot plate
150 DEG C of temperature.
Using fire-retardant made from the method/antibiotic multifunction polyester fiber filament number:1.5 ~ 2.5dtex, fracture strength
>=3.5CN/dtex, elongation at break >=15%, line density deviation ratio ± 7.0;By obtained fiber woven into fabric, according to GB/
T5454-1997《Textile combustion performance test oxygen index method》Measure the LOI of the fire-retardant/antibiotic multifunction Polyester Fibers
For 30%, the antibiotic rate 99.9% of Escherichia coli.
Embodiment 5
By 750g polyester master particles, 7g micro-nano montmorillonite powders, particle diameter is less than 200 nanometers of 5 grams of silica, 8 grams of red phosphorus, neatly
8 grams of stone, 6g glass fibres carry silver-colored 37.5 grams of silicate, 2.60g silane couplers KH570,0.5g light stabilizer, 2g antioxidant,
2.5g stearic acid, 6g atoleines add high mixer, with standby after 750rpm rotating speed mixing 7min.
By in above-mentioned well mixed raw material input double screw extruder, the design temperature in the area of twin-screw one to No.12 District is
190-215 DEG C, die head sets 210 DEG C, screw speed 170rpm, and feeding frequency is 7Hz.
(2)By obtained fire-retardant/antibiotic multifunction polyester master particle at 100 DEG C forced air drying 2 hours, then put
Enter in vacuum drying chamber 125 DEG C of dryings 48 hours, be cooled to 40 DEG C, add ethylene bis stearic acid amide and obtain spinning material, institute
The addition for stating ethylene bis stearic acid amide is the 0.8wt% of spinning material, and spinning material is added in melt spinning machine and spun
Silk, 265 DEG C of spinning temperature, spinning winding speed are 800m/min, obtained nascent fire resistance fibre, on Barmag drafting machines
First break draft processing is carried out, obtains fire-retardant/antibiotic multifunction polyester fiber, wherein 3 times of drafting multiple, 60 DEG C of temperature of heat plate, hot plate
140 DEG C of temperature.
Using fire-retardant made from the method/antibiotic multifunction polyester fiber filament number:1.5 ~ 3.0dtex, fracture strength
>=3.0CN/dtex, elongation at break >=20%, line density deviation ratio ± 8.0;By obtained fiber woven into fabric, according to GB/
T5454-1997《Textile combustion performance test oxygen index method》Measure the LOI of the fire-retardant/antibiotic multifunction Polyester Fibers
For 29%, the antibiotic rate of Escherichia coli is 99%.
Claims (10)
1. a kind of polyester-base nano hydridization is fire-retardant/preparation method of antibiotic multifunction fiber, it is characterised in that:
(1)By dried polyester master particle, including montmorillonite, the compound resistance of inorganic nano fire retardant, hydrotalcite and glass fibre
Agent, inorganic nano antiseptic, coupling agent, light, oxygen stabilizer, including the lubricant of stearic acid and atoleine are fired, by following matter
Amount is added in high-speed mixer and is well mixed:
1 750 grams of polyester master particle
24 ~ 10 grams of montmorillonites
3 13 ~ 40 grams of inorganic nano fire retardants
4 1.5-10 grams of hydrotalcites
54 ~ 15 grams of glass fibres
6 7.5 ~ 37.5 grams of inorganic nano antiseptics
7 2.12 ~ 3.18 grams of coupling agents
8 0.5 gram of light stabilizers
92 grams of antioxidants
10 2 grams of stearic acid ~ 3 grams
11 6 grams of atoleines ~ 8 grams;
(2)Under the conditions of 30-180 DEG C, the compound that stirs and evenly mixs, under the conditions of 240-300 DEG C, double screw extruder is put into
In, melt blending extruding pelletization, obtain fire-retardant/antibiotic multifunction complex polyester master batch;So that the addition of composite flame-retardant agent is
The 3-10wt% of polyester, the addition of inorganic nano antiseptic are the 1-5wt% of polyester, wherein, the process conditions of twin-screw extrusion
For:The design temperature of an area to No.12 District is set between 160-220 DEG C of scope, 200-220 DEG C of die temperature, screw rod
Rotating speed 100-200rpm, feeding frequency are 6-12Hz;
(3)Above-mentioned polyester composite master batch is dried, is subsequently cooled to 40-90 DEG C, adds dispersant, obtains spinning original
Material, spinning is carried out, drawing-off processing, produces fire-retardant/antibiotic multifunction composite polyester fiber, the wherein addition of dispersant is spinning
The 0.1-2wt% of raw material.
2. the polyester-base nano hydridization according to claim 1 is fire-retardant/preparation method of antibiotic multifunction fiber, its feature exists
In:Step(1)In, the inorganic nano fire retardant be particle diameter less than 200 nanometers aluminum oxide, magnesia, silica, red phosphorus,
One or more in expanded graphite;Described glass fibre is the glass fibre that draw ratio is more than 10.
3. the polyester-base nano hydridization according to claim 1 is fire-retardant/preparation method of antibiotic multifunction fiber, its feature exists
In:Step(1)In, inorganic nano antiseptic is the one or more in silver-loaded zirconium phosphate, the silver-colored glass of load, load silver silicate.
4. according to the polyester-base nano hydridization of claims 1 or 2 it is fire-retardant/preparation method of antibiotic multifunction fiber, it is special
Sign is:Step(1)In, described coupling agent is titanate coupling agent and/or silane coupler.
5. the polyester-base nano hydridization according to claim 1 is fire-retardant/preparation method of antibiotic multifunction fiber, its feature exists
In:The step(2)Middle dry polyester composite master batch method is:Forced air drying 1-5h, is then put at 80-140 DEG C
Enter 110-170 DEG C of dry 12-60h in vacuum drying chamber.
6. the polyester-base nano hydridization according to claim 1 is fire-retardant/preparation method of antibiotic multifunction fiber, its feature exists
In:The step(2)Middle dispersant is one or both of pentaerythritol stearate, ethylene bis stearic acid amide.
7. the polyester-base nano hydridization according to claim 1 is fire-retardant/preparation method of antibiotic multifunction fiber, its feature exists
In:The step(3)Middle spinning technology parameter is:Composite spinning machine carries out spinning, 240-300 DEG C of spinning temperature, spinning winding
Speed is 600-3000m/min.
8. the polyester-base nano hydridization according to claim 1 is fire-retardant/preparation method of antibiotic multifunction fiber, its feature exists
In:The step(3)Middle drawing-off machined parameters are 1-3.5 times of drafting multiple, 50-90 DEG C of temperature of heat plate, hot plate temperature 120-
200℃。
9. a kind of polyester-base nano hydridization is fire-retardant/antibiotic multifunction fiber, it is characterised in that according to claim 1-8 is any
Method is prepared.
10. application of the polyester-base nano hydridization multifunctional fibre in fire-retardant/antibacterial according to claim 9.
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CN109957223A (en) * | 2019-03-28 | 2019-07-02 | 中国科学院长春应用化学研究所 | A kind of nano combined spinning material of inorganic nano tripoli modified PBT and preparation method thereof |
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CN112981594A (en) * | 2021-02-14 | 2021-06-18 | 碧金美 | Antibacterial waterproof functional polyester fabric |
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CN109168312A (en) * | 2018-08-06 | 2019-01-08 | 佛山市南海区佳妍内衣有限公司 | The electromagnetic shielding fiber cloth being made of glass fibre |
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CN112981594A (en) * | 2021-02-14 | 2021-06-18 | 碧金美 | Antibacterial waterproof functional polyester fabric |
CN113774510A (en) * | 2021-08-26 | 2021-12-10 | 浙江恒澜科技有限公司 | Preparation method of expanded graphite polyester flame-retardant fabric |
CN113774510B (en) * | 2021-08-26 | 2023-05-12 | 浙江恒逸石化研究院有限公司 | Preparation method of expanded graphite polyester flame-retardant fabric |
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Application publication date: 20180130 |