CN110003624A - A kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic and preparation method thereof - Google Patents
A kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08L2201/02—Flame or fire retardant/resistant
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- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a kind of HI high impacts, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic and preparation method thereof.This PBT plastic includes: PBT15~43%；PET4~10%；MCA4~10%；Decabromodiphenylethane 5~7%；Brominated Polystyrene 5~7%；Sodium antimonate 0.5~3%；TPP2~5%；EMA-g-GMA 3~10%；EBA-g-GMA 3~10%；Antioxidant 0.3~1%；Lubricant 0.3~1%；Glass fibre 18~25%.The preparation method of this PBT plastic is also disclosed simultaneously.PBT plastic of the present invention is compounded using polynary fire retardant and polynary toughener, it can reduce the dosage of fire retardant while improving flame retarding efficiency, the impact resistance of material is improved simultaneously, the requirement of 850 DEG C of the nonflammable temperature of glowing filament can not only be reached, and material has high impact property, meets harsh job requirements.
Description
Technical field
The invention belongs to polymeric material fields, enhance PBT plastic more particularly to a kind of HI high impact, high-glowing-filament-temperature flame-retardancy
And preparation method thereof.
Background technique
Polybutylene terephthalate (PBT), English name polybutylene terephthalate (abbreviation PBT) are a kind of
Thermoplastic polyester is developed in the last century initial stage seventies by Celanese company, the U.S..PBT has extraordinary heat-resisting
Property, weatherability, chemical-resistant, and have many advantages, such as that excellent electric properties, water imbibition are small, surface is good, it is widely used
In the industries such as electric, automobile, machinery, household electrical appliance, especially electric industry.
Normally, electric industry has flame-retardancy requirements to material mostly, generally requires the whole nonflammable temperature of glowing filament
Up to 750 DEG C.The PBT material of early stage is modified by adding a large amount of fire retardant, and the whole nonflammable temperature of glowing filament can reach 750
℃.With the development of society, electronic product is increasingly intended to high-end development, European electronic product to the standard of PBT material again
A step is improved, 850 DEG C are risen to by original 750 DEG C to the nonflammable temperature of glowing filament.However, according to traditional improvement
Method continues to add fire retardant on PBT material of the nonflammable temperature of glowing filament up to 750 DEG C, although can make the glowing filament of PBT material
Nonflammable temperature is up to 850 DEG C, but the mechanical property of material can completely lose, without practical application value.For example, existing use bromine
It is compound for triazine, antimony oxide, MCA fire retardant (Chinese name: melamine cyanurate), the flame retardant property of PBT material is improved,
But the PBT material mechanical property obtained is excessively poor.Moreover, because fire retardant additive amount is big, pulvis is untreated to be directly added into,
Processing technology is caused to be difficult to control.In addition, fire retardant compounding type is few, flame retarding efficiency, glowing filament efficiency are low, therefore additive amount
Greatly, and brominated triazine it is expensive, lead to higher cost, be not suitable for practical application.Therefore, flame-retardant PBT material how is taken into account
Mechanical property and glowing filament performance, become row in worker concern hot issue.
Summary of the invention
Of the existing technology in order to overcome the problems, such as, one of the objects of the present invention is to provide a kind of HI high impacts, Gao Zhuore
Silk flame-retardant reinforced PBT plastic, the second object of the present invention are to provide this HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic
Preparation method.
The present invention is compounded by polynary fire retardant and polynary toughener, can reduce while improving flame retarding efficiency
The dosage of fire retardant examines this flame-retardant reinforced PBT plastic according to GB/T1843 to improve the impact resistance of PBT material
IZOD impact strength >=15KJ/m of survey2(i.e. HI high impact), and the fire-retardant requirement for reaching 850 DEG C of the nonflammable temperature of glowing filament is (i.e.
High glow-wire).
In order to achieve the above purpose, the technical solution used in the present invention is:
The present invention provides a kind of HI high impact, high-glowing-filament-temperature flame-retardancies to enhance PBT plastic, the original including following mass percent
Expect component:
Polybutylene terephthalate (PBT) 15%~43%；
Polyethylene terephthalate 4%~10%；
Melamine cyanurate 4%~10%；
Decabromodiphenylethane 5%~7%；
Brominated Polystyrene 5%~7%；
Sodium antimonate 0.5%~3%；
Triphenyl phosphate 2%~5%；
Ethylene-methyl acrylate copolymer graft glycidyl methacrylate 3%~10%；
Ethylene-butyl acrylate copolymer graft glycidyl methacrylate 3%~10%；
Antioxidant 0.3%~1%；
Lubricant 0.3%~1%；
Glass fibre 18%~25%.
In this HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic, the preferred quality hundred of polybutylene terephthalate (PBT)
Divide than being 35%~42%；The preferred mass percent of polyethylene terephthalate is 4%~6%；Cyanuric acid melamine
The preferred mass percent of amine is 4%~6%；The preferred mass percent of sodium antimonate is 0.5%~2%；Triphenyl phosphate is excellent
The mass percent of choosing is 2%~4%；Ethylene-methyl acrylate copolymer graft glycidyl methacrylate is preferred
Mass percent is 4%~6%；The preferred quality of ethylene-butyl acrylate copolymer graft glycidyl methacrylate
Percentage is 6%~8%；The preferred mass percent of antioxidant is 0.4%~0.8%；The preferred mass percent of lubricant
It is 0.4%~0.8%；The preferred mass percent of glass fibre is 19%~22%.
In the present invention, relevant Name Resolution is as follows:
Polybutylene terephthalate (PBT): PBT；
Polyethylene terephthalate；PET；
Melamine cyanurate: MCA；
Triphenyl phosphate: TPP；
Ethylene-methyl acrylate copolymer graft glycidyl methacrylate: EMA-g-GMA；
Ethylene-butyl acrylate copolymer graft glycidyl methacrylate: EBA-g-GMA.
Preferably, this HI high impact, high-glowing-filament-temperature flame-retardancy enhance in PBT plastic, the spy of polybutylene terephthalate (PBT)
Property viscosity be 0.9dl/g~1.1dl/g；Use the polybutylene terephthalate (PBT) resin of the intrinsic viscosity range, Ke Yibao
Demonstrate,prove the mobility and performance of material.
Preferably, this HI high impact, high-glowing-filament-temperature flame-retardancy enhance in PBT plastic, the spy of polyethylene terephthalate
Property viscosity be 0.6dl/g~0.7dl/g；Use the pet resin of the intrinsic viscosity range, Ke Yibao
Demonstrate,prove the mobility and performance of material.
Preferably, this HI high impact, high-glowing-filament-temperature flame-retardancy enhance in PBT plastic, and melamine cyanurate is through silane idol
Join the melamine cyanurate of agent surface treatment；The phase of melamine cyanurate and PBT after silane coupling agent is surface-treated
Capacitive is more preferable.
Preferably, this HI high impact, high-glowing-filament-temperature flame-retardancy enhance in PBT plastic, and antioxidant is Hinered phenols antioxidant, Asia
At least one of phosphoric acid ester antioxidant；Hinered phenols antioxidant can be selected from antioxidant 245,264,1010,1024,1076,
At least one of 1098；Phosphite ester antioxidant can be selected from least one of irgasfos 168,626；Further preferably
, antioxidant is one of antioxidant 1010,168 or combinations thereof object.
Preferably, this HI high impact, high-glowing-filament-temperature flame-retardancy enhance in PBT plastic, and lubricant is selected from silicone powder, fatty acid acyl
Amine, stearic acid, stearate, paraffin, polyethylene wax, erucyl amide, oleamide, ethylene bis stearic acid amide (EBS), Ji Wusi
At least one of double stearates (PETS) of alcohol；It is further preferred that lubricant is selected from the double stearic acid acyls of silicone powder, ethylene
At least one of double stearates of amine, pentaerythrite；Still further preferably, lubricant is silicone powder.
The present invention also provides this HI high impacts, the preparation method of high-glowing-filament-temperature flame-retardancy enhancing PBT plastic, including following step
It is rapid:
1) raw material is weighed according to above-mentioned composition；
2) by melamine cyanurate, decabromodiphenylethane, brominated Polystyrene, sodium antimonate, triphenyl phosphate, antioxidant
And mix lubricant, obtain builder granule；
3) by builder granule and polybutylene terephthalate (PBT), polyethylene terephthalate, ethylene-acrylic acid first
Ester copolymer graft glycidyl methacrylate, ethylene-butyl acrylate copolymer grafted methacrylic acid glycidol
Ester mixing, obtains mixture；
4) mixture and glass fibre are subjected to melting extrusion, are granulated, obtain HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT
Plastics.
Preferably, this HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic preparation method step 2) in, mixing be
Revolving speed is that 3min~10min is stirred in the blender of 400r/min~800r/min.
Preferably, this HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic preparation method step 3) in, mixing be
Revolving speed is that 5min~8min is stirred in the blender of 100r/min~300r/min.
Preferably, this HI high impact, high-glowing-filament-temperature flame-retardancy enhance in the preparation method step 4) of PBT plastic, melting extrusion
It is to be carried out in double screw extruder.
The beneficial effects of the present invention are:
PBT plastic of the invention is compounded using polynary fire retardant and polynary toughener, while improving flame retarding efficiency
It can reduce the dosage of fire retardant, while improving the impact resistance of material, the nonflammable temperature 850 of glowing filament can not only be reached
DEG C requirement, and material has high impact property, meets harsh job requirements.
Compared with prior art, advantages of the present invention is specific as follows:
1, the fire retardant of PBT material of the invention addition is can to significantly improve PBT line made of polynary fire retardant compounding
Efficiency while improving the glow wire temperature of PBT, guarantees that the mechanical property of PBT plastic can satisfy requirement.
2, the present invention selects polynary toughener to be compounded, right while efficiently improving the shock resistance of material
Anti-flammability influences smaller.
3, MCA of the invention passes through silane coupling agent surface preparation, preferable with PBT compatibility after processing.
4, preparation method of the invention uses powder auxiliary pretreatment mode, powder is first become " particle ", reduces processing
Shi Fenmo separates bring unstability with particle.
Specific embodiment
The contents of the present invention are described in further detail below by way of specific embodiment.Raw material used in example
Unless otherwise specified, it can be obtained from routine business approach.
Embodiment 1
A kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhance PBT plastic, the raw material components including following mass percent:
PBT 41%；
PET 5%；
MCA 5%；
Decabromodiphenylethane 5%；
Brominated Polystyrene 7%；
Sodium antimonate 1%；
TPP 3%；
EMA-g-GMA 6%；
EBA-g-GMA 6%；
Antioxidant 0.5%；
Lubricant 0.5%；
Glass fibre 20%.
The inherent viscosity of PBT used in this example is 0.9~1.1dl/g.The inherent viscosity of PET is 0.6~0.7dl/g.
MCA is the MCA by silane coupling agent surface preparation.Antioxidant used is antioxidant 1010 and irgasfos 168 with quality
Than the compound antioxidant of 3:2 composition.Lubricant used is silicone powder.
This HI high impact of this example, high-glowing-filament-temperature flame-retardancy enhance the preparation method of PBT plastic, comprising the following steps:
1) raw material is weighed according to above-mentioned composition；
2) by decabromodiphenylethane, brominated Polystyrene, sodium antimonate, MCA, TPP, antioxidant 1010, irgasfos 168 and silicon
Ketone powder stirs 5min in 600r/min stirrer for mixing, and TPP is bundled together with other auxiliary agents, forms granular auxiliary agent
Grain；
3) builder granule and PBT, PET, EMA-g-GMA, EBA-g-GMA are stirred in 200r/min stirrer for mixing
6min obtains mixture；
4) double screw extruder is used, mixture and glass fibre are subjected to melting extrusion, is granulated, obtains HI high impact, height
Glowing filament flame-retardant reinforced PBT plastic.
Embodiment 2
A kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhance PBT plastic, the raw material components including following mass percent:
PBT 41%；
PET 5%；
MCA 5%；
Decabromodiphenylethane 7%；
Brominated Polystyrene 5%；
Sodium antimonate 1%；
TPP 3%；
EMA-g-GMA 6%；
EBA-g-GMA 6%；
Antioxidant 0.5%；
Lubricant 0.5%；
Glass fibre 20%.
Raw material type and preparation method and embodiment 1 used in this example HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic
It is identical.
Embodiment 3
A kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhance PBT plastic, the raw material components including following mass percent:
PBT 41%；
PET 5%；
MCA 5%；
Decabromodiphenylethane 7%；
Brominated Polystyrene 5%；
Sodium antimonate 1%；
TPP 3%；
EMA-g-GMA 4%；
EBA-g-GMA 8%；
Antioxidant 0.5%；
Lubricant 0.5%；
Glass fibre 20%.
Raw material type and preparation method and embodiment 1 used in this example HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic
It is identical.
Comparative example 1
A kind of PBT plastic, the raw material components including following mass percent:
PBT 41%；
PET 5%；
MCA 5%；
Decabromodiphenylethane 12%；
Sodium antimonate 1%；
TPP 3%；
EMA-g-GMA 6%；
EBA-g-GMA 6%；
Antioxidant 0.5%；
Lubricant 0.5%；
Glass fibre 20%.
Raw material type used in this example PBT plastic is identical as embodiment 1.
The PBT plastic preparation method of this example compared with Example 1, only difference is that and be added without brominated Polystyrene,
Remaining preparation method is all the same.
Comparative example 2
A kind of PBT plastic, the raw material components including following mass percent:
PBT 41%；
PET 5%；
MCA 5%；
Brominated Polystyrene 12%；
Sodium antimonate 1%；
TPP 3%；
EMA-g-GMA 6%；
EBA-g-GMA 6%；
Antioxidant 0.5%；
Lubricant 0.5%；
Glass fibre 20%.
Raw material type used in this example PBT plastic is identical as embodiment 1.
The PBT plastic preparation method of this example compared with Example 1, only difference is that and be added without decabromodiphenylethane,
Remaining preparation method is all the same.
Comparative example 3
A kind of PBT plastic, the raw material components including following mass percent:
PBT 41%；
PET 5%；
MCA 5%；
Decabromodiphenylethane 5%；
Brominated Polystyrene 7%；
Sodium antimonate 1%；
TPP 3%；
EBA-g-GMA 12%；
Antioxidant 0.5%；
Lubricant 0.5%；
Glass fibre 20%.
Raw material type used in this example PBT plastic is identical as embodiment 1.
The PBT plastic preparation method of this example compared with Example 1, only difference is that and be added without EMA-g-GMA, remaining system
Preparation Method is all the same.
Comparative example 4
A kind of PBT plastic, the raw material components including following mass percent:
PBT 41%；
PET 5%；
MCA 5%；
Decabromodiphenylethane 5%；
Brominated Polystyrene 7%；
Sodium antimonate 1%；
TPP 3%；
EMA-g-GMA 12%；
Antioxidant 0.5%；
Lubricant 0.5%；
Glass fibre 20%.
Raw material type used in this example PBT plastic is identical as embodiment 1.
The PBT plastic preparation method of this example compared with Example 1, only difference is that and be added without EBA-g-GMA, remaining system
Preparation Method is all the same.
Comparative example 5
It is formed according to the raw material of embodiment 1, builder granule first is not made in powder auxiliary, but according to common mixing side
Method is mixed with.As a result, it has been found that blanking is unstable during production, production technology is difficult to control.
PBT plastic made from Examples 1 to 3 and comparative example 1~4 is tested for the property, wherein Mechanics Performance Testing
Environment is: 23 DEG C, dry state.The test result of Examples 1 to 3 is shown in Table 1, and the test result of comparative example 1~4 is shown in Table 2.
The PBT plastic test result of 1 Examples 1 to 3 of table
The PBT plastic test result of 2 comparative example 1~4 of table
By the test result comparison of Tables 1 and 2 it is found that the exclusive use of comparative example 1 decabromodiphenylethane is at high cost, and draws
It is relatively low to stretch intensity bending strength；Brominated Polystyrene is used alone in comparative example 2, and glow wire temperature is relatively low；Comparative example 3 is used alone
EMA-g-GMA, at high cost, good impact resistance, but influence glowing filament；EBA-g-GMA impact resistance is used alone slightly in comparative example 4
Difference.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhance PBT plastic, it is characterised in that: the raw material including following mass percent
Component:
Polybutylene terephthalate (PBT) 15%~43%；
Polyethylene terephthalate 4%~10%；
Melamine cyanurate 4%~10%；
Decabromodiphenylethane 5%~7%；
Brominated Polystyrene 5%~7%；
Sodium antimonate 0.5%~3%；
Triphenyl phosphate 2%~5%；
Ethylene-methyl acrylate copolymer graft glycidyl methacrylate 3%~10%；
Ethylene-butyl acrylate copolymer graft glycidyl methacrylate 3%~10%；
Antioxidant 0.3%~1%；
Lubricant 0.3%~1%；
Glass fibre 18%~25%.
2. a kind of HI high impact according to claim 1, high-glowing-filament-temperature flame-retardancy enhance PBT plastic, it is characterised in that: described poly-
The inherent viscosity of mutual-phenenyl two acid bromide two alcohol ester is 0.9dl/g~1.1dl/g.
3. a kind of HI high impact according to claim 1, high-glowing-filament-temperature flame-retardancy enhance PBT plastic, it is characterised in that: described poly-
The inherent viscosity of ethylene glycol terephthalate is 0.6dl/g~0.7dl/g.
4. a kind of HI high impact according to claim 1, high-glowing-filament-temperature flame-retardancy enhance PBT plastic, it is characterised in that: the cyanogen
Uric acid melamine is the melamine cyanurate being surface-treated through silane coupling agent.
5. a kind of HI high impact according to claim 1, high-glowing-filament-temperature flame-retardancy enhance PBT plastic, it is characterised in that: described anti-
Oxygen agent is at least one of Hinered phenols antioxidant, phosphite ester antioxidant.
6. a kind of HI high impact according to claim 1, high-glowing-filament-temperature flame-retardancy enhance PBT plastic, it is characterised in that: the profit
Lubrication prescription is selected from silicone powder, fatty acid amide, stearic acid, stearate, paraffin, polyethylene wax, erucyl amide, oleamide, ethylene
At least one of double stearates of double stearic amides, pentaerythrite.
7. the preparation method of a kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic, it is characterised in that: the following steps are included:
1) raw material is weighed according to the described in any item compositions of claim 1~6；
2) by melamine cyanurate, decabromodiphenylethane, brominated Polystyrene, sodium antimonate, triphenyl phosphate, antioxidant and profit
Lubrication prescription mixing, obtains builder granule；
3) builder granule and polybutylene terephthalate (PBT), polyethylene terephthalate, ethylene-methyl acrylate is total
Polymers graft glycidyl methacrylate, ethylene-butyl acrylate copolymer graft glycidyl methacrylate are mixed
It closes, obtains mixture；
4) mixture and glass fibre are subjected to melting extrusion, are granulated, obtain HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic.
8. according to claim 7 a kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic preparation method, feature exists
In: in step 2), mixing is that 3min~10min is stirred in the blender that revolving speed is 400r/min~800r/min.
9. according to claim 7 a kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic preparation method, feature exists
In: in step 3), mixing is that 5min~8min is stirred in the blender that revolving speed is 100r/min~300r/min.
10. according to claim 7 a kind of HI high impact, high-glowing-filament-temperature flame-retardancy enhancing PBT plastic preparation method, feature exists
In: in step 4), melting extrusion is carried out in double screw extruder.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112063128A (en) * | 2020-09-16 | 2020-12-11 | 佛山市汉纬新材料有限公司 | High-glow-wire impact-resistant high-fluidity reinforced flame-retardant PBT (polybutylene terephthalate) material and preparation method thereof |
| CN112143181A (en) * | 2020-09-24 | 2020-12-29 | 广州市聚赛龙工程塑料股份有限公司 | Highlight high glow wire reinforced flame-retardant PBT (polybutylene terephthalate) composite material as well as preparation method and application thereof |
| CN114031908A (en) * | 2022-01-11 | 2022-02-11 | 广东顺德顺炎新材料股份有限公司 | Polyethylene glycol terephthalate modified engineering plastic and preparation method thereof |
| CN115304895A (en) * | 2022-08-31 | 2022-11-08 | 芜湖聚发新材料有限公司 | Reinforced flame-retardant PBT (polybutylene terephthalate) material and manufacturing method thereof |
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| CN112063128A (en) * | 2020-09-16 | 2020-12-11 | 佛山市汉纬新材料有限公司 | High-glow-wire impact-resistant high-fluidity reinforced flame-retardant PBT (polybutylene terephthalate) material and preparation method thereof |
| CN112143181A (en) * | 2020-09-24 | 2020-12-29 | 广州市聚赛龙工程塑料股份有限公司 | Highlight high glow wire reinforced flame-retardant PBT (polybutylene terephthalate) composite material as well as preparation method and application thereof |
| CN112143181B (en) * | 2020-09-24 | 2022-08-16 | 广州市聚赛龙工程塑料股份有限公司 | Highlight high glow wire reinforced flame-retardant PBT (polybutylene terephthalate) composite material as well as preparation method and application thereof |
| CN114031908A (en) * | 2022-01-11 | 2022-02-11 | 广东顺德顺炎新材料股份有限公司 | Polyethylene glycol terephthalate modified engineering plastic and preparation method thereof |
| CN115304895A (en) * | 2022-08-31 | 2022-11-08 | 芜湖聚发新材料有限公司 | Reinforced flame-retardant PBT (polybutylene terephthalate) material and manufacturing method thereof |
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