CN108912549A - A kind of highly effective flame-retardant type PVC floor and preparation method thereof - Google Patents
A kind of highly effective flame-retardant type PVC floor and preparation method thereof Download PDFInfo
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- CN108912549A CN108912549A CN201810790975.7A CN201810790975A CN108912549A CN 108912549 A CN108912549 A CN 108912549A CN 201810790975 A CN201810790975 A CN 201810790975A CN 108912549 A CN108912549 A CN 108912549A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of 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 a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Health & Medical Sciences (AREA)
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Abstract
The present invention provides a kind of highly effective flame-retardant type PVC floor and preparation method thereof, and the highly effective flame-retardant type PVC floor includes the raw material of following parts by weight：80~120 parts of PVC, 0.5~2 part of orthophosphoric acid melamine, 2~12 parts of phenyl boric acid pinacol ester, 1~2 part of sucrose fatty ester, 2~8 parts of octamethylcy-clotetrasiloxane, 1~3 part of Compritol 888 ATO, 2~5 parts of nonyl phenol modifying benzoxazine resin, 0.5~1.5 part of light stabilizer；The preparation method of the highly effective flame-retardant type PVC floor includes the following steps：S1, raw material is weighed；The modification of S2, phenyl boric acid pinacol ester and sucrose fatty ester to orthophosphoric acid melamine；The mixing of S3, raw material；S4, plasticate, pressing mold, cooling, mould unloading is up to highly effective flame-retardant type PVC floor.PVC floor proposed by the present invention, rationally, processing forming, resistance to ag(e)ing and good flame resistance, excellent in mechanical performance is low cigarette, nontoxic, environmental-friendly for formula.
Description
Technical field
The present invention relates to technical field of floor more particularly to a kind of highly effective flame-retardant type PVC floor and preparation method thereof.
Background technique
The primary raw material that PVC floor uses is polyvinyl chloride, and polyvinyl chloride is environmentally friendly, nontoxic, renewable resource, therefore
PVC floor is safe and environment-friendly, and in addition to this PVC floor also has many advantages, such as light, high resiliency and high-impact.But traditional PVC
Plate flame retardant property is poor, there is security risk in use, or even can expand the intensity of a fire.In order to improve the fire-retardant of PVC floor
Characteristic, it will usually fire retardant is added into PVC floor material, common fire retardant mainly has halogenated flame retardant, inorganic fire retardants
And phosphorus flame retardant.Since halogenated flame retardant can generate toxic gas in use, gradually used by limitation, and
The usually bigger mechanical property that can deteriorate PVC floor of the dosage of inorganic fire retardants influences the service life of PVC floor, the resistance of phosphorus system
The flame retardant effect of combustion agent increases compared to inorganic fire retardants, but the usage amount of phosphorus flame retardant is still larger, and phosphorus system hinders
Agent meeting acidic materials during fire-retardant are fired, PVC floor material is caused to corrode.Based on the deficiencies in the prior art, originally
Invention proposes a kind of highly effective flame-retardant type PVC floor and preparation method thereof.
Summary of the invention
The purpose of the present invention is to solve the flame retardant property of existing PVC floor is bad, the fire retardant of flame retardant type PVC floor
Additive amount is big, it is difficult to the problem of dispersing and easily deteriorating PVC mechanical property, corrosion easily is caused to material, and the one kind proposed is efficiently
Flame retardant type PVC floor and preparation method thereof.
In order to achieve the above object, the present invention is achieved by the following technical programs：
A kind of highly effective flame-retardant type PVC floor, the raw material including following parts by weight：80~120 parts of PVC, orthophosphoric acid melamine
0.5~2 part, 2~12 parts of phenyl boric acid pinacol ester, 1~2 part of sucrose fatty ester, eight 2~8 parts of urgent cyclotetrasiloxanes, behenyl
1~3 part of acid glyceride, 2~5 parts of nonyl phenol modifying benzoxazine resin, 0.5~1.5 part of light stabilizer.
Preferably, the highly effective flame-retardant type PVC floor includes the raw material of following parts by weight：90~110 parts of PVC, orthophosphoric acid
0.8~1.6 part of melamine, 2.4~9.6 parts of phenyl boric acid pinacol ester, 1.2~1.6 parts of sucrose fatty ester, prestox ring four
3~7 parts of siloxanes, 1.5~2.5 parts of Compritol 888 ATO, 3~4.5 parts of nonyl phenol modifying benzoxazine resin, light stabilizer
0.8~1.2 part.
Preferably, the mass ratio of the phenyl boric acid pinacol ester and sucrose fatty ester is 2~6：1, it is further preferred that
The mass ratio of the phenyl boric acid pinacol ester and sucrose fatty ester is 4：1.
Preferably, the highly effective flame-retardant type PVC floor includes the raw material of following parts by weight：100 parts of PVC, orthophosphoric acid trimerization
1.2 parts of cyanamide, 5.6 parts of phenyl boric acid pinacol ester, 1.4 parts of sucrose fatty ester, 5 parts of octamethylcy-clotetrasiloxane, behenic acid are sweet
2 parts of grease, 4 parts of nonyl phenol modifying benzoxazine resin, 1 part of light stabilizer.
Preferably, light stabilizer is poly-succinic (4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine ethanols) ester and 2- cyanogen
The mixture of base -3,3 diphenylacrylate ethyl alcohol, and poly-succinic (4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine ethanols) ester
Mass ratio with 2- cyano -3,3 diphenylacrylate ethyl alcohol is 2：3.
The invention also provides a kind of preparation methods of highly effective flame-retardant type PVC floor, include the following steps：
S1, according to 80~120 parts of PVC, 0.5~2 part of orthophosphoric acid melamine, 2~12 parts of phenyl boric acid pinacol ester, Sucrose Fatty Acid Ester
1~2 part of fat acid esters, eight 2~8 parts of urgent cyclotetrasiloxanes, 1~3 part of Compritol 888 ATO, nonyl phenol modifying benzoxazine resin
2~5 parts, 0.5~1.5 part of light stabilizer weigh each raw material, spare；
S2, the in the mixed solvent that the weighed phenyl boric acid pinacol ester of step S1 and sucrose fatty ester are added to 5 times of quality, in
40 DEG C of concussions disperse 30min, and 20min is stirred under the revolving speed of 200r/min, are concentrated under reduced pressure, and are dried in vacuo to get composite powder
Then the weighed orthophosphoric acid melamine of step S1 and composite powder are added in the ethyl alcohol of 5 times of amounts, in 400r/min's by end
20min is stirred under revolving speed, then recycling ethyl alcohol is concentrated under reduced pressure to get modified orthophosphoric acid melamine；
S3, by the weighed PVC of step S1, eight urgent cyclotetrasiloxanes, Compritol 888 ATO, nonyl phenol modified benzoxazine tree
The modification orthophosphoric acid melamine that rouge, light stabilizer and step S2 are prepared is added in high-speed mixer, is uniformly mixed
And room temperature is down to up to total mixture；
S4, it total mixture is put into plasticator plasticates, carry out pressing mold, cooling, mould unloading then up to highly effective flame-retardant type PVC
Floor.
Preferably, it is 7 that the mixed solvent, which is volume ratio,：3 ethyl alcohol and the mixture of ether.
Highly effective flame-retardant type PVC floor provided by the invention, advantage is compared with prior art：
1, PVC floor proposed by the present invention, formula rationally, using PVC as major ingredient, pass through addition octamethylcy-clotetrasiloxane, behenyl
Acid glyceride, nonyl phenol modifying benzoxazine resin and light stabilizer, to improve processing forming, the resistance to ag(e)ing of PVC floor
And the dispersibility of each raw material, and assigned by addition orthophosphoric acid melamine, phenyl boric acid pinacol ester, sucrose fatty ester
PVC excellent flame-retarding characteristic effectively overcomes traditional PVC floor flame retardant property bad, the fire retardant additive amount of flame retardant type PVC floor
Greatly, it is difficult to which the problem of dispersing and easily deteriorating PVC mechanical property, easily cause corrosion to material, in addition to this, the present invention is prepared
The low cigarette of PVC floor, nontoxic, environmental-friendly.
2, the present invention is modified orthophosphoric acid melamine by phenyl boric acid pinacol ester and sucrose fatty ester, can
Enhance the reactivity of orthophosphoric acid melamine, improve the binding force of orthophosphoric acid melamine and PVC, and positive phosphorus can be significantly improved
The flame retardant effect of sour melamine reduces the usage amount of orthophosphoric acid melamine, reduces fire retardant additive amount greatly to PVC floor power
The influence of performance is learned, and the stability of orthophosphoric acid melamine can also be improved, proposes the decomposition temperature of orthophosphoric acid melamine
It is high by 12%, effectively overcome the problems, such as that traditional melamine substance meets high temperature and easily decomposes generation noxious material, and the experiment proved that change
Property orthophosphoric acid melamine be added can phenyl boric acid pinacol ester and sucrose fatty ester there is synergistic function, especially
Be the mass ratio of phenyl boric acid pinacol ester and sucrose fatty ester be 4：When 1, the flame retardant property and mechanical property of PVC floor are most
Excellent, oxygen index (OI) can achieve 45.3%；
3, the preparation method of highly effective flame-retardant type PVC floor proposed by the present invention, easy to operate, the good mixing effect between raw material,
First phenyl boric acid pinacol ester and sucrose fatty ester are compounded in the in the mixed solvent formed with ethyl alcohol and ether, then will
To composite powder be modified in ethanol with orthophosphoric acid melamine, modified orthophosphoric acid melamine is prepared, finally
Modified orthophosphoric acid melamine is mixed with other raw materials in PVC floor again, is formed, can be improved orthophosphoric acid melamine
Reactivity, make the PVC floor oxygen index (OI) being prepared improve 4%.
Specific embodiment
Combined with specific embodiments below the present invention is made further to explain.
A kind of preparation method of highly effective flame-retardant type PVC floor proposed by the present invention, includes the following steps：
S1, it is weighed according to the parts by weight of each raw material in table 1, it is spare；
S2, the in the mixed solvent that the weighed phenyl boric acid pinacol ester of step S1 and sucrose fatty ester are added to 5 times of quality are mixed
Bonding solvent is that volume ratio is 7：3 ethyl alcohol and the mixture of ether, and disperse 30min in 40 DEG C of concussions, then at 200r/min's
20min is stirred under revolving speed, is concentrated under reduced pressure, and is dried in vacuo to get composite powder, then by the weighed orthophosphoric acid melamine of step S1
Amine and composite powder are added in the ethyl alcohol of 5 times of amounts, 20min are stirred under the revolving speed of 400r/min, then recycling second is concentrated under reduced pressure
Alcohol is to get modified orthophosphoric acid melamine；
S3, by the weighed PVC of step S1, octamethylcy-clotetrasiloxane, Compritol 888 ATO, nonyl phenol modified benzoxazine tree
The modification orthophosphoric acid melamine that rouge, light stabilizer and step S2 are prepared is added in high-speed mixer, is uniformly mixed
And room temperature is down to up to total mixture；
S4, it total mixture is put into plasticator plasticates, carry out pressing mold, cooling, mould unloading then up to highly effective flame-retardant type PVC
Floor.
Performance detection is carried out to the above-mentioned highly effective flame-retardant type PVC floor being prepared, the results are shown in Table 2.
Table 1：The parts by weight of each raw material in embodiment
| Component | A | B | C | D | E | F | G | H |
| Embodiment 1 | 80 | 0.5 | 2 | 1 | 2 | 1 | 2 | 0.5 |
| Embodiment 2 | 100 | 1.2 | 5.6 | 1.4 | 5 | 2 | 4 | 1 |
| Embodiment 3 | 120 | 2 | 12 | 2 | 8 | 3 | 5 | 1.5 |
| Comparative example 1 | 120 | 2 | 0 | 14 | 8 | 3 | 5 | 1.5 |
| Comparative example 2 | 120 | 2 | 14 | 0 | 8 | 3 | 5 | 1.5 |
| Comparative example 3 | 120 | 2 | 4.7 | 9.3 | 8 | 3 | 5 | 1.5 |
| Comparative example 4 | 120 | 2 | 5.6 | 8.4 | 8 | 3 | 5 | 1.5 |
| Embodiment 4 | 120 | 2 | 7 | 7 | 8 | 3 | 5 | 1.5 |
| Embodiment 5 | 120 | 2 | 8.4 | 5.6 | 8 | 3 | 5 | 1.5 |
| Embodiment 6 | 120 | 2 | 9.3 | 4.7 | 8 | 3 | 5 | 1.5 |
| Embodiment 7 | 120 | 2 | 10.5 | 3.5 | 8 | 3 | 5 | 1.5 |
| Embodiment 8 | 120 | 2 | 11.2 | 2.8 | 8 | 3 | 5 | 1.5 |
| Embodiment 9 | 120 | 2 | 11.7 | 2.3 | 8 | 3 | 5 | 1.5 |
| Embodiment 10 | 120 | 2 | 12 | 2 | 8 | 3 | 5 | 1.5 |
| Embodiment 11 | 120 | 2 | 12.25 | 1.75 | 8 | 3 | 5 | 1.5 |
| Embodiment 12 | 120 | 2 | 12.44 | 1.56 | 8 | 3 | 5 | 1.5 |
| Embodiment 13 | 120 | 2 | 12.73 | 1.27 | 8 | 3 | 5 | 1.5 |
| Embodiment 14 | 120 | 2 | 12.92 | 1.08 | 8 | 3 | 5 | 1.5 |
| Comparative example 5 | 120 | 2 | 13 | 1 | 8 | 3 | 5 | 1.5 |
| Comparative example 6 | 120 | 2 | 13.07 | 0.93 | 8 | 3 | 5 | 1.5 |
In table 1, A PVC, B are positive melamine phosphate, and C is phenyl boric acid pinacol ester, and D is sucrose fatty ester, and E is eight first
Basic ring tetrasiloxane, F are Compritol 888 ATO, and G is nonyl phenol modifying benzoxazine resin, and H is light stabilizer, and light stabilizer is
Poly-succinic (4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine ethanols) ester and 2- cyano -3,3 diphenylacrylate ethyl alcohol it is mixed
Close object, and poly-succinic (4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine ethanols) ester and 2- cyano -3,3 diphenylacrylate second
The mass ratio of alcohol is 2：3.
Table 2：The PVC floor the performance test results of embodiment preparation
| Test item | Tensile strength（MPa） | Oxygen index (OI)（%） | Smoke density |
| Embodiment 1 | 43.6 | 38.2 | 114 |
| Embodiment 2 | 55.2 | 45.3 | 109 |
| Embodiment 3 | 45.9 | 40.1 | 112 |
| Comparative example 1 | 21.7 | 26.6 | 123 |
| Comparative example 2 | 19.8 | 27.5 | 119 |
| Comparative example 3 | 21.5 | 29.2 | 116 |
| Comparative example 4 | 23.6 | 29.7 | 111 |
| Embodiment 4 | 32.8 | 31.6 | 115 |
| Embodiment 5 | 35.6 | 32.7 | 112 |
| Embodiment 6 | 44.2 | 38.5 | 109 |
| Embodiment 7 | 46.6 | 40.6 | 110 |
| Embodiment 8 | 54.6 | 44.1 | 109 |
| Embodiment 9 | 47.4 | 41.8 | 106 |
| Embodiment 11 | 37.8 | 36.5 | 111 |
| Embodiment 12 | 35.7 | 34.9 | 115 |
| Embodiment 13 | 34.9 | 33.7 | 116 |
| Embodiment 14 | 33.7 | 32.3 | 114 |
| Comparative example 5 | 24.4 | 29.4 | 110 |
| Comparative example 6 | 22.9 | 28.9 | 109 |
According to the test result of Examples 1 to 3 in table 2 show PVC floor proposed by the present invention have good mechanical property and
Excellent anti-flammability, and smoke amount is small；
Show benzene boron in PVC floor proposed by the present invention according to the test result of embodiment 3, comparative example 1 and comparative example 2 in table 2
Sour pinacol ester and sucrose fatty ester compounding are modified obtained mechanical property and anti-flammability to orthophosphoric acid melamine
It can be better than phenyl boric acid pinacol ester or sucrose fatty ester obtained PVC cyanurotriamide modified to orthophosphoric acid is used alone
Plate；
According to embodiment 3, comparative example 3, comparative example 4 in table 2, the test result of comparative example 5 and comparative example 6 shows when in formula
The mass ratio of phenyl boric acid pinacol ester and sucrose fatty ester is less than 1:1 or be greater than 12:1 obtained PVC floor it is fire-retardant
Performance and mechanical property improvement are not obvious；When in formula the mass ratio of phenyl boric acid pinacol ester and sucrose fatty ester be 1~
12：When between 1, the oxygen index (OI) and tensile strength for the PVC floor being prepared improve, and comprehensive performance is more excellent；Especially
The mass ratio for being phenyl boric acid pinacol ester and sucrose fatty ester is 2~6:When between 1, the oxygen for the PVC floor being prepared refers to
Several and tensile strength tool increases significantly, and is 4 in the mass ratio of phenyl boric acid pinacol ester and sucrose fatty ester：When 1, system
Standby obtained PVC floor oxygen index (OI) is up to that 44.1%, tensile strength is up to 54.6MPa, smoke density only has 109, and comprehensive performance is most
It is excellent.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of highly effective flame-retardant type PVC floor, which is characterized in that the raw material including following parts by weight：80~120 parts of PVC, just
0.5~2 part of melamine phosphate, 2~12 parts of phenyl boric acid pinacol ester, 1~2 part of sucrose fatty ester, eight urgent four silicon oxygen of ring
2~8 parts of alkane, 1~3 part of Compritol 888 ATO, 2~5 parts of nonyl phenol modifying benzoxazine resin, 0.5~1.5 part of light stabilizer.
2. a kind of highly effective flame-retardant type PVC floor according to claim 1, which is characterized in that the original including following parts by weight
Material：90~110 parts of PVC, 0.8~1.6 part of orthophosphoric acid melamine, 2.4~9.6 parts of phenyl boric acid pinacol ester, sucrose-fatty
1.2~1.6 parts of ester, 3~7 parts of octamethylcy-clotetrasiloxane, 1.5~2.5 parts of Compritol 888 ATO, nonyl phenol modified benzoxazine
3~4.5 parts of resin, 0.8~1.2 part of light stabilizer.
3. a kind of highly effective flame-retardant type PVC floor according to claim 1 or 2, which is characterized in that the phenyl boric acid pinacol
The mass ratio of ester and sucrose fatty ester is 2~6：1.
4. a kind of highly effective flame-retardant type PVC floor according to claim 1 or 2, which is characterized in that including following parts by weight
Raw material：100 parts of PVC, 1.2 parts of orthophosphoric acid melamine, 5.6 parts of phenyl boric acid pinacol ester, 1.4 parts of sucrose fatty ester, eight first
5 parts of basic ring tetrasiloxane, 2 parts of Compritol 888 ATO, 4 parts of nonyl phenol modifying benzoxazine resin, 1 part of light stabilizer.
5. a kind of highly effective flame-retardant type PVC floor according to claim 1 or 2, which is characterized in that the light stabilizer is poly-
The mixing of succinic acid (4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine ethanols) ester and 2- cyano -3,3 diphenylacrylate ethyl alcohol
Object, and poly-succinic (4- hydroxyl -2,2,6,6- tetramethyl -1- piperidine ethanols) ester and 2- cyano -3,3 diphenylacrylate ethyl alcohol
Mass ratio be 2：3.
6. a kind of preparation method of highly effective flame-retardant type PVC floor, which is characterized in that include the following steps：
S1, according to 80~120 parts of PVC, 0.5~2 part of orthophosphoric acid melamine, 2~12 parts of phenyl boric acid pinacol ester, Sucrose Fatty Acid Ester
1~2 part of fat acid esters, eight 2~8 parts of urgent cyclotetrasiloxanes, 1~3 part of Compritol 888 ATO, nonyl phenol modifying benzoxazine resin
2~5 parts, 0.5~1.5 part of light stabilizer weigh each raw material, spare；
S2, the in the mixed solvent that the weighed phenyl boric acid pinacol ester of step S1 and sucrose fatty ester are added to 5 times of quality, in
40 DEG C of concussions disperse 30min, and 20min is stirred under the revolving speed of 200r/min, are concentrated under reduced pressure, and are dried in vacuo to get composite powder
Then the weighed orthophosphoric acid melamine of step S1 and composite powder are added in the ethyl alcohol of 5 times of amounts, in 400r/min's by end
20min is stirred under revolving speed, then recycling ethyl alcohol is concentrated under reduced pressure to get modified orthophosphoric acid melamine；
S3, by the weighed PVC of step S1, eight urgent cyclotetrasiloxanes, Compritol 888 ATO, nonyl phenol modified benzoxazine tree
The modification orthophosphoric acid melamine that rouge, light stabilizer and step S2 are prepared is added in high-speed mixer, is uniformly mixed
And room temperature is down to up to total mixture；
S4, it total mixture is put into plasticator plasticates, carry out pressing mold, cooling, mould unloading then up to highly effective flame-retardant type PVC
Floor.
7. a kind of preparation method of highly effective flame-retardant type PVC floor according to claim 6, which is characterized in that the mixing
Solvent is that volume ratio is 7：3 ethyl alcohol and the mixture of ether.
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Application publication date: 20181130 |