CN109721967A - A kind of polyester material bright in luster and preparation method thereof - Google Patents

A kind of polyester material bright in luster and preparation method thereof Download PDF

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Publication number
CN109721967A
CN109721967A CN201711060711.8A CN201711060711A CN109721967A CN 109721967 A CN109721967 A CN 109721967A CN 201711060711 A CN201711060711 A CN 201711060711A CN 109721967 A CN109721967 A CN 109721967A
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parts
temperature
area
ethylene
polyester material
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杨桂生
杨莺
李术
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Hefei Genius New Materials Co Ltd
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Hefei Genius New Materials Co Ltd
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Abstract

The invention belongs to technical field of polymer materials, more particularly to a kind of bright polyester material and preparation method thereof, the polyester material is prepared by weight by following components: 42-82 parts of polyester terephthalate, 5-40 parts of ethylene-octene copolymer, ethylene-methyl methacrylate butyl ester -3-10 parts of glycidyl acrylate, synergistic colour reinforcing agent 3-10 parts, 0.5-5 parts of color master-batch, 0.1-0.5 parts of antioxidant, 0.1-1.0 parts of lubricant.The present invention is used using color master-batch, synergistic coloring reinforcing agent collaboration, whole to have extraordinary colorability, good toner dispersibility while material keeps mechanics stability.Products of the present invention is bright-colored, is evenly distributed, and property retention is good, has good color homogeneity.

Description

A kind of polyester material bright in luster and preparation method thereof
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of bright polyester material and its preparation side Method.
Background technique
With the development of technology, the polyester terephthalate class material in thermoplastic polyester is on automobile using increasingly wider It is general.Wherein being modified polybutylene terephthalate (PBT) (abbreviation PBT) plastics is most important car light material, it can not only subtract The quality of light components about 40%, but also purchase cost can be made to reduce by 40% or so, therefore its dosage in the car is fast Speed rises.In addition, PBT has good comprehensive performance, and such as high-fire resistance, toughness, fatigue durability, self-lubricating, low-friction coefficient, Weatherability, water absorption rate are low etc..But the volume resistance of PBT is big, dielectric loss is big, and notch impact strength is low, and molding shrinkage is big. And polyethylene terephthalate (abbreviation PET) is the polymer of highly crystalline, smooth surface is glossy, in wider temperature There is excellent physical mechanical property, for long-term use temperature up to 120 DEG C, electrical insulating property is excellent, or even in high temperature height in range Under frequency, electrical property is still preferable, but corona resistance is poor, creep resistance, fatigue durability, and rub resistance, dimensional stability are all very It is good.
So meet the needs of final component and client to promote material property and class, it is general by enhancing, filling out It the methods of fills, be blended and improve its processability and modification, resin rigidity, heat resistance, resistance to chemical reagents, electric property and weather-proof can be improved Property.With continually developing for application, people propose higher, more specific requirement to polyester, for example, color of the people for product Coloured silk has more pursuits, and this requires rapidoprints to have the advantages that easy dyeing.Since toner holds very much in enhancing system Easily there is the problem of color divergence unevenness, and since the addition of toner is easy so that the performance decline of material is obvious.Therefore, it opens Sending out the evenly dispersed method of modification technology and pigment of the bright-coloured polyester material to polyester a kind of proposes the comprehensive performance of modified poly ester It rises, technological improvement and practical application are of great significance.
Summary of the invention
The object of the present invention is to provide a kind of bright polyester materials and preparation method thereof.
In order to achieve the object of the present invention, it the present invention provides a kind of bright polyester material, is pressed by following components Parts by weight are prepared:
Further scheme, the polyester terephthalate are polybutylene terephthalate (PBT) (PBT) or poly- terephthaldehyde Sour glycol ester (PET).
The inherent viscosity of the polybutylene terephthalate (PBT) (PBT) is 0.5-1.5dl/g, and described is poly- to benzene two Formic acid glycol ester (PET) inherent viscosity is 0.6-1.0dl/g.
The ethylene-octene copolymer is to compound toughening with ethylene-methyl methacrylate butyl ester-glycidyl acrylate Agent.The effect of compounding, better than single toughening effect.
The synergistic coloring reinforcing agent is inorganic crystal whisker.
The inorganic crystal whisker is by the mixture that calcium carbonate crystal whisker and calcium sulfate crystal whiskers are that 10:1 is formed in mass ratio.
The color master-batch is made of by weight following components:
100 parts of ultra-low viscosity PET
0-25 parts of titanium dioxide
0-2 parts of blue or green blue
0-2 parts of dark green
0-5 parts of titanium yellow powder
0.01-1 parts of carbon black
0-2 parts of iron oxide red.
The inherent viscosity 0.5dl/g of the ultra-low viscosity PET, the carbon black are activating surface free flowing black.
The antioxidant is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters and three (2,4- Di-tert-butyl-phenyl) phosphite ester mixture;The lubricant is silicone powder.
Another goal of the invention of the invention is to provide a kind of preparation method of bright polyester material comprising with Lower step:
(1) by 100 parts of ultra-low viscosity PET, 0-25 parts of titanium dioxide, 0-2 parts of blue or green blue, 0-2 parts of dark green, titanium yellow powder 0-5 Part, 0.01-1 parts of carbon black and 0-2 parts of iron oxide red obtain color master-batch through mixing, extruding pelletization;
(2) dried following components is weighed: 42-82 parts of polyester terephthalate, 5-40 parts of ethylene-octene copolymer, Ethylene-methyl methacrylate butyl ester -3-10 parts of glycidyl acrylate, synergistic colour reinforcing agent 3-10 parts, color master-batch 0.5-5 Part, 0.1-0.5 parts of antioxidant, 0.1-1.0 parts of lubricant;
(3) by the polyester terephthalate weighed up, ethylene-methyl methacrylate butyl ester-glycidyl acrylate, synergistic Color reinforcing agent, ethylene-octene copolymer, color master-batch, antioxidant and lubricant pass through mixed with 600r/min in high-speed mixer Close 2~10min;The raw material mixed is added in double screw extruder, is granulated through melting extrusion, is made bright poly- Ester material;One area's temperature of double screw extruder is 200-230 DEG C, and two area's temperature are 200-230 DEG C, and three area's temperature are 200- 240 DEG C, four area's temperature are 210-240 DEG C, and five area's temperature are 210-250 DEG C, and six area's temperature are 220-250 DEG C;Twin-screw host Revolving speed is 250-500rpm.
Beneficial effects of the present invention:
Each component coordinative role and its processing technology ensure that the workability and toner polymolecularity of color master-batch.
The present invention is used using color master-batch, synergistic coloring reinforcing agent collaboration, and material keeps the same of mechanics stability When, making material integrally has extraordinary colorability, good toner dispersibility.
Products of the present invention is bright-colored, is evenly distributed, and property retention is good, has good color homogeneity.
Specific embodiment
The following describes the present invention further through the description of specific embodiments, but it is to limit of the invention that this, which is not, System, those skilled in the art's basic thought according to the present invention can make various modifications or improvements, but without departing from this The basic thought of invention, is all within the scope of the present invention.
The inherent viscosity of polybutylene terephthalate (PBT) (PBT) is 0.5-1.5dl/g, the poly terephthalic acid second Diol ester (PET) inherent viscosity is 0.6-1.0dl/g.
Carbon black is activating surface free flowing black.
Synergistic coloring reinforcing agent is by the mixture that calcium carbonate crystal whisker and calcium sulfate crystal whiskers are that 10:1 is formed in mass ratio.
Testing standard:
Physical property Test method
Tensile strength ASTM D638
Izod notch impact strength (izodtest) ASTM D256
Bending strength ASTM D790
Bending modulus ASTM D790
Toner disperses (tinting strength, tinting power) grade UL94 range estimation
Embodiment 1
(1) preparation of color master-batch: by 100 parts of ultra-low viscosity PET, 25 parts of titanium dioxide, 1.5 parts of blue or green blue, carbon black 0.01 Part, 1.5 parts of iron oxide red, high-speed mixer is added and is uniformly mixed, then extruding pelletization obtains color master-batch in double screw extruder; The wherein processing conditions of double screw extruder are as follows: area's temperature is 200 DEG C, and two area's temperature are 205 DEG C, and three area's temperature are 210 DEG C, Four area's temperature are 220 DEG C, and five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C;Twin-screw engine speed is 300rpm.
(2) dried following components is weighed by mass parts: 62 parts of PET, 25 parts of ethylene-octene copolymer, ethylene-first 5 parts of base butylacrylate-acrylic acid ethylene oxidic ester, synergistic colour 5 parts of reinforcing agent, 3 parts of color master-batch, 0.1 part of antioxidant, moisten 0.5 part of lubrication prescription;
(3) by the PET weighed up, ethylene-octene copolymer, ethylene-methyl methacrylate butyl ester-glycidyl acrylate, Synergistic colours reinforcing agent, color master-batch, antioxidant and lubricant and is uniformly mixed by high-speed mixer, speed of agitator 600r/ Min, incorporation time 2min;Then the raw material mixed is added in double screw extruder, is granulated through melting extrusion, color is made Color bright-coloured polyester material.The processing conditions of double screw extruder are as follows: area's temperature be 200 DEG C, two area's temperature be 205 DEG C, three Area's temperature is 210 DEG C, and four area's temperature are 220 DEG C, and five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C;Twin-screw engine speed For 300rpm.
Embodiment 2
(1) preparation of color master-batch: by ultralow 100 parts of viscous PET, 25 parts of titanium dioxide, 2 parts of blue or green blue, 1 part of carbon black, iron oxide red 2 parts, 2 parts of dark green, 5 parts of addition high-speed mixers of titanium yellow powder are uniformly mixed, and then extruding pelletization obtains in double screw extruder To color master-batch.The processing conditions of double screw extruder are as follows: area's temperature is 200 DEG C, and two area's temperature are 205 DEG C, three Qu Wendu It is 210 DEG C, four area's temperature are 220 DEG C, and five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C;Twin-screw engine speed is 300rpm。
(2) preparation of bright-coloured polyester material: dried following components is weighed by mass parts: 62 parts of PET, ethylene-octene 25 parts of copolymer, ethylene-methyl methacrylate butyl ester -5 parts of glycidyl acrylate, synergistic colours 5 parts of reinforcing agent, color master-batch 3 parts, 0.1 part of antioxidant, 0.5 part of lubricant;The polyester that will be weighed up, ethylene-methyl methacrylate butyl ester-glycidyl Ester, ethylene-octene copolymer, synergistic colour reinforcing agent, and color master-batch, antioxidant, lubricant is mixed equal by high-speed mixer It is even, speed of agitator 600r/min, 2~10min of incorporation time;The raw material mixed is added in double screw extruder, is passed through Melting extrusion is granulated, and bright-coloured polyester material is made.The processing conditions of double screw extruder are as follows: area's temperature is 200 DEG C, two area's temperature Degree is 205 DEG C, and three area's temperature are 210 DEG C, and four area's temperature are 220 DEG C, and five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C;It is double Screw host revolving speed is 300rpm.
Embodiment 3
(1) preparation of color master-batch: by ultralow 100 parts of viscous PET, 15 parts of titanium dioxide, 0.5 part of dark green, 1.0 parts of iron oxide red, 0.01 part of addition high-speed mixer of carbon black is uniformly mixed, and then extruding pelletization obtains color master-batch in double screw extruder.It is double The processing conditions of screw extruder are as follows: area's temperature is 200 DEG C, and two area's temperature are 205 DEG C, and three area's temperature are 210 DEG C, four Qu Wen Degree is 220 DEG C, and five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C;Twin-screw engine speed is 300rpm.
(2) preparation of bright-coloured polyester material: dried following components is weighed by mass parts: 42 parts of polyester, ethylene-octene 40 parts of copolymer, ethylene-methyl methacrylate butyl ester -3 parts of glycidyl acrylate, synergistic colour 10 parts of reinforcing agent, color masterbatch 5 parts, 0.5 part of antioxidant, 1.0 parts of lubricant of grain;The polyester that will be weighed up, ethylene-octene copolymer, ethylene-methyl methacrylate fourth Ester-glycidyl acrylate, synergistic colour reinforcing agent, and color master-batch, antioxidant, lubricant is mixed equal by high-speed mixer It is even, speed of agitator 600r/min, 2~10min of incorporation time;The raw material mixed is added in double screw extruder, is passed through Melting extrusion is granulated, and bright-coloured polyester material is made.The processing conditions of double screw extruder are as follows: area's temperature is 230 DEG C, two area's temperature Degree is 230 DEG C, and three area's temperature are 240 DEG C, and four area's temperature are 240 DEG C, and five area's temperature are 250 DEG C, and six area's temperature are 250 DEG C;It is double Screw host revolving speed is 500rpm.
Embodiment 4
(1) preparation of color master-batch: by ultralow 100 parts of viscous PET, 10 parts of titanium dioxide, 2.5 parts of titanium yellow powder, 0.5 part of iron oxide red, 0.01 part of addition high-speed mixer of carbon black is uniformly mixed, and then extruding pelletization obtains color master-batch in double screw extruder.It is double The processing conditions of screw extruder are as follows: area's temperature is 200 DEG C, and two area's temperature are 205 DEG C, and three area's temperature are 210 DEG C, four Qu Wen Degree is 220 DEG C, and five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C;Twin-screw engine speed is 300rpm.
(2) preparation of bright-coloured polyester material: dried following components is weighed by mass parts: 82 parts of polyester, ethylene-octene 5 parts of copolymer, ethylene-methyl methacrylate butyl ester -10 parts of glycidyl acrylate, synergistic colours 3 parts of reinforcing agent, color master-batch 0.5 part, 0.3 part of antioxidant, 0.1 part of lubricant;The polyester that will be weighed up, ethylene-octene copolymer, ethylene-methyl methacrylate fourth Ester-glycidyl acrylate, synergistic colour reinforcing agent, and color master-batch, antioxidant, lubricant is mixed equal by high-speed mixer It is even, speed of agitator 600r/min, 2~10min of incorporation time;The raw material mixed is added in double screw extruder, is passed through Melting extrusion is granulated, and bright-coloured polyester material is made.The processing conditions of double screw extruder are as follows: area's temperature is 210 DEG C, two area's temperature Degree is 215 DEG C, and three area's temperature are 220 DEG C, and four area's temperature are 230 DEG C, and five area's temperature are 240 DEG C, and six area's temperature are 250 DEG C;It is double Screw host revolving speed is 250rpm.
Comparative example 1
Difference with embodiment 1 is that toner auxiliary agent is not made into color master-batch.
Weigh dried following components by mass parts: PET64.3436 parts, 25 parts of ethylene-octene copolymer, ethylene-first 5 parts of base butylacrylate-acrylic acid ethylene oxidic ester, 5 parts of reinforcing agent of synergistic coloring, 0.5859 part of titanium dioxide, blue or green blue 0.0352 part, 0.0002 part of carbon black, 0.0352 part of iron oxide red, 0.1 part of antioxidant, 0.5 part of lubricant;The polyester that will be weighed up, ethylene- Octene copolymer, ethylene-methyl methacrylate butyl ester-glycidyl acrylate, synergistic coloring reinforcing agent, titanium dioxide, blue or green blue, Carbon black, iron oxide red, antioxidant, lubricant are uniformly mixed by high-speed mixer, speed of agitator 600r/min, and incorporation time 2~ 10min;The raw material mixed is added in double screw extruder, is granulated through melting extrusion, bright-coloured polyester material is made.Double spiral shells The processing conditions of bar extruder are as follows: area's temperature is 200 DEG C, and two area's temperature are 205 DEG C, and three area's temperature are 210 DEG C, four Qu Wendu It is 220 DEG C, five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C;Twin-screw engine speed is 300rpm.
Comparative example 2
Difference with embodiment 1 is not plus synergistic colours reinforcing agent:
(1) preparation of color master-batch: by ultralow 100 parts of viscous PET, 25 parts of titanium dioxide, 1.5 parts of blue or green blue, carbon black 0.01 Part, 1.5 parts of iron oxide red, high-speed mixer is added and is uniformly mixed, then extruding pelletization obtains color master-batch in double screw extruder. The processing conditions of double screw extruder are as follows: area's temperature is 200 DEG C, and two area's temperature are 205 DEG C, and three area's temperature are 210 DEG C, 4th area Temperature is 220 DEG C, and five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C;Twin-screw engine speed is 300rpm.
(2) preparation of polyester material: dried following components is weighed by mass parts: 62 parts of PET, ethylene-octene is copolymerized 25 parts of object, ethylene-methyl methacrylate butyl ester -5 parts of glycidyl acrylate, 3 parts of color master-batch, 0.1 part of antioxidant, lubricant 0.5 part;The polyester that will be weighed up, ethylene-octene copolymer, ethylene-methyl methacrylate butyl ester-glycidyl acrylate, coloring Master batch, antioxidant, lubricant are uniformly mixed by high-speed mixer, speed of agitator 600r/min, 2~10min of incorporation time; The raw material mixed is added in double screw extruder, is granulated through melting extrusion, bright-coloured polyester material is made.Twin-screw extrusion The processing conditions of machine are as follows: area's temperature is 200 DEG C, and two area's temperature are 205 DEG C, and three area's temperature are 210 DEG C, and four area's temperature are 220 DEG C, five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C;Twin-screw engine speed is 300rpm.
Comparative example 3
With embodiment 1 difference be toner auxiliary agent be not made into color master-batch and not plus synergistic coloring reinforcing agent:
Weigh dried following components by mass parts: PET64.3436 parts, 25 parts of ethylene-octene copolymer, ethylene-first 5 parts of base butylacrylate-acrylic acid ethylene oxidic ester, 0.5859 part of titanium dioxide, 0.0352 part of blue or green blue, 0.0002 part of carbon black, 0.0352 part of iron oxide red, 0.1 part of antioxidant, 0.5 part of lubricant;The polyester that will be weighed up, ethylene-octene copolymer, ethylene-methyl-prop Olefin(e) acid butyl ester-glycidyl acrylate, titanium dioxide, blue or green blue, carbon black, iron oxide red, antioxidant, lubricant pass through high-speed mixer It is uniformly mixed, speed of agitator 600r/min, 2~10min of incorporation time;The raw material mixed is added to double screw extruder In, it is granulated through melting extrusion, bright-coloured polyester material is made.The processing conditions of double screw extruder are as follows: area's temperature is 200 DEG C, Two area's temperature are 205 DEG C, and three area's temperature are 210 DEG C, and four area's temperature are 220 DEG C, and five area's temperature are 220 DEG C, and six area's temperature are 225 ℃;Twin-screw engine speed is 300rpm.
Above-described embodiment 1-4 and comparative example 1-3 polyester material prepared is molded into accordingly according to GB testing standard respectively Batten is tested after then placing 24 hours in the environment of 23 ± 2 DEG C, 50 ± 5% relative humidity, and performance test is as follows:
1 performance data of table
It can be seen that from the performance comparison of upper table embodiment 1-4 and comparative example 1-3, the present invention is by the way that toner auxiliary agent to be improved to Color master-batch form, while the addition of synergistic coloring reinforcing agent, while effectively keeping the mechanical property of polyester product, favorably In the coloring of color master-batch, make that product colour is bright-coloured, is evenly distributed.
The present invention is not limited to the above embodiments, and those skilled in the art's announcement according to the present invention is not departing from the present invention The improvement and modification that scope is made all should be within protection scope of the present invention.

Claims (10)

1. a kind of bright polyester material, which is characterized in that be prepared by weight by following components:
42-82 parts of polyester terephthalate,
5-40 parts of ethylene-octene copolymer,
Ethylene-methyl methacrylate butyl ester -3-10 parts of glycidyl acrylate,
Synergistic colours reinforcing agent 3-10 parts,
0.5-5 parts of color master-batch,
0.1-0.5 parts of antioxidant,
0.1-1.0 parts of lubricant.
2. a kind of bright polyester material according to claim 1, it is characterised in that: the polyester terephthalate For polybutylene terephthalate (PBT) or polyethylene terephthalate.
3. a kind of bright polyester material according to claim 2, it is characterised in that: the poly terephthalic acid fourth The inherent viscosity of diol ester is 0.5-1.5dl/g, and the polyethylene terephthalate inherent viscosity is 0.6-1.0 dl/g.
4. a kind of bright polyester material according to claim 1, it is characterised in that: the synergistic colours enhancing Agent is inorganic crystal whisker.
5. a kind of bright polyester material according to claim 4, it is characterised in that: the inorganic crystal whisker be by Calcium carbonate crystal whisker and calcium sulfate crystal whiskers are the mixture of 10:1 composition in mass ratio.
6. a kind of bright polyester material according to claim 1, which is characterized in that the color master-batch is under Component is stated to form by weight:
100 parts of ultra-low viscosity polyethylene terephthalate,
0-25 parts of titanium dioxide,
0-2 parts of blue or green blue,
0-2 parts of dark green,
0-5 parts of titanium yellow powder,
0.01-1 parts of carbon black,
0-2 parts of iron oxide red.
7. a kind of bright polyester material according to claim 1, it is characterised in that: poly- pair of the ultra-low viscosity 0.5 dl/g of inherent viscosity of ethylene terephthalate, the carbon black are activating surface free flowing black.
8. a kind of bright polyester material according to claim 1, it is characterised in that: the antioxidant is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester and three (2,4- di-tert-butyl-phenyl) phosphite esters Mixture;The lubricant is silicone powder.
9. a kind of preparation method of the described in any item bright polyester materials of claim 1 ~ 8, which is characterized in that including Following steps:
(1) by 100 parts of ultra-low viscosity polyethylene terephthalate, 0-25 parts of titanium dioxide, 0-2 parts of blue or green blue, dark green 0-2 Part, 0-5 parts of titanium yellow powder, 0.01-1 parts of carbon black and 0-2 parts of iron oxide red obtain color master-batch through mixing, extruding pelletization;
(2) dried following components is weighed: 42-82 parts of polyester terephthalate, 5-40 parts of ethylene-octene copolymer, ethylene- Butyl methacrylate -3-10 parts of glycidyl acrylate, synergistic colour reinforcing agent 3-10 parts, 0.5-5 parts of color master-batch, resist 0.1-0.5 parts of oxygen agent, 0.1-1.0 parts of lubricant;
(3) polyester terephthalate weighed up, ethylene-methyl methacrylate butyl ester-glycidyl acrylate, synergistic coloring are increased Strong agent, ethylene-octene copolymer, color master-batch, antioxidant and lubricant by high-speed mixer with 600r/min mixing 2~ 10min;The raw material mixed is added in double screw extruder, is granulated through melting extrusion, bright polyester material is made Material.
10. a kind of preparation method of bright polyester material according to claim 9, it is characterised in that: step (3) One area's temperature of double screw extruder is 200-230 DEG C, and two area's temperature are 200-230 DEG C, and three area's temperature are 200-240 DEG C, Four area's temperature are 210-240 DEG C, and five area's temperature are 210-250 DEG C, and six area's temperature are 220-250 DEG C;Twin-screw engine speed is 250-500rpm。
CN201711060711.8A 2017-10-31 2017-10-31 A kind of polyester material bright in luster and preparation method thereof Pending CN109721967A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112375345A (en) * 2020-10-29 2021-02-19 金发科技股份有限公司 Laser marking shading enhanced PBT composition and preparation method and application thereof

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Application publication date: 20190507