CN109777056A - A kind of melt-drip resistant inflaming retarding polyester composite and its preparation method and application - Google Patents
A kind of melt-drip resistant inflaming retarding polyester composite and its preparation method and application Download PDFInfo
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- CN109777056A CN109777056A CN201910124096.5A CN201910124096A CN109777056A CN 109777056 A CN109777056 A CN 109777056A CN 201910124096 A CN201910124096 A CN 201910124096A CN 109777056 A CN109777056 A CN 109777056A
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- fire retardant
- inflaming retarding
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- drip resistant
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Abstract
The present invention provides a kind of melt-drip resistant inflaming retarding polyester composites and its preparation method and application.Melt-drip resistant inflaming retarding polyester composite of the present invention is mainly made of the following raw material: PET resin, bridge chain DOPO derivative species fire retardant and anti-dropping agent；The bridge chain DOPO derivative species fire retardant includes formula (I) structural compounds.In the present invention, bridge chain DOPO derivative species fire retardant and polyester material compatibility are good, a small amount of anti-dripping agent is added by synergistic compounding, prepared polyester composite excellent fireproof performance, polyester material molten drop phenomenon be improved significantly, the vertical combustion grade of composite material can be widely used for the field having higher requirements to flame retardant property up to UL94V-0, flame retardant polyester composite material prepared by the present invention.
Description
Technical field
The present invention relates to high molecular material field of fire-proof technology, compound in particular to a kind of melt-drip resistant inflaming retarding polyester
Material and its preparation method and application.
Background technique
Polyethylene terephthalate (PET) is a kind of high molecular polymerization for being widely used in fiber and non-fiber field
Object material.As it is in the extension of the application fields such as automobile, electronic apparatus material, household items, building, to the peace of PET material
The requirement of full performance especially flame retardant property is higher and higher.
Currently, phosphonium flame retardant or phosphorus-nitrogen combustion inhibitor are effective fire retardants of PET.But pure PET material is being burnt
In the process, hardly at charcoal, fusing flowing is serious, and melt drip phenomenon is serious.The harmfulness of high temperature molten drop can not be ignored, melting
Drippage normally results in spot fire and the direct injury to human body.Therefore, the high temperature molten drop of PET is the skill that polyester flame-retardant faces
Art problem, this makes polyester material receive certain limitation in flame retardant area use.
Existing polyester is mainly to pass through the drippage of molten drop to take away heat to realize fire-retardant purpose with phosphonium flame retardant, because
This is the high temperature molten drop problem for being difficult to solve PET material if only adding existing phosphonium flame retardant.
In view of this, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of melt-drip resistant inflaming retarding polyester composite, and melt-drip resistant inflaming retarding of the present invention is poly-
Ester composite material not only has good flame retardant property, but also is able to suppress the high temperature molten drop of PET.
The second object of the present invention is to provide a kind of preparation method of melt-drip resistant inflaming retarding polyester composite.
The third object of the present invention is to provide a kind of application of melt-drip resistant inflaming retarding polyester composite.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A kind of melt-drip resistant inflaming retarding polyester composite, the melt-drip resistant inflaming retarding polyester composite is mainly by the following raw material system
At: PET resin, bridge chain DOPO derivative species fire retardant and anti-dropping agent；
Wherein, the bridge chain DOPO derivative species fire retardant includes such as following formula (I) structural compounds:
Wherein, in formula (I), l, m are independently the integer more than or equal to 0；Condition is that l, m are not 0 simultaneously；L1For
Chemical bond, C1-C12Linear chain or branched chain alkylidene, C5-C30Arlydene or C5-C30Heteroarylidene；Condition is to work as L1
When not being chemical bond, L1Upper arbitrary hydrogen atom is optional substituted or non-substituted.
Meanwhile the present invention also provides the preparation methods of the melt-drip resistant inflaming retarding polyester composite, comprising: by PET
Resin and bridge chain DOPO derivative species fire retardant, anti-dropping agent carry out melt blending processing after evenly mixing, obtain anti-dropping resistance
Retardant polyester composite material.
Further, present invention provides the melt-drip resistant inflaming retarding polyester composites in fibrous material or electronics electricity
Application in device；And/or application of the melt-drip resistant inflaming retarding polyester composite in communications and transportation；And/or
Person, application of the melt-drip resistant inflaming retarding polyester composite in decorative building material field.
Compared with prior art, the invention has the benefit that
In the present invention, using the DOPO derivative containing phenyl ring as fire retardant, it can not only be shown with PET material well
Compatibility, and since in DOPO derivative, containing the benzene ring structure that connects to group, PET composite material can be increased
Layer of charcoal, synergistic adds a small amount of anti-dripping agent in addition, so as to press down while guaranteeing the flame retardant property of PET composite material
The high temperature molten drop phenomenon of PET processed.
Preparation method simple process of the present invention, operating condition is mild, is suitable for industrialization large-scale production.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific
Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is
The conventional products that can be obtained by commercially available purchase.
Melt-drip resistant inflaming retarding polyester composite provided by the present invention is in view of existing PET fire proofing anti-dropping performance
It is insufficient and proposition, by using the DOPO derivative compound for having phenyl ring as fire retardant and anti-on a small quantity melt of arranging in pairs or groups in the present invention
Drops so that melt-drip resistant inflaming retarding polyester composite of the present invention can not only keep good mechanical performance, while also having
There is excellent anti-fire and is able to suppress the high temperature molten drop of PET resin.
Specifically, melt-drip resistant inflaming retarding polyester composite provided by the present invention is by PET resin, bridge chain DOPO derivative
Based flame retardant and anti-dropping agent are made of raw material；
Wherein, (a) PET resin:
In the present invention, raw materials used PET resin is any commercially available or other synthesis PET resins.
(b) bridge chain DOPO derivative species fire retardant:
DOPO derivative flame retardant with phenyl is used in PET resin system be one of main points of the invention, specifically
, the bridge chain DOPO derivative species flame retardant mechanism is as follows:
Wherein, in formula (I), l, m are independently the integer more than or equal to 0；
Condition is that l, m are not 0 simultaneously, i.e. l >=0, m >=0, and l+m >=1；
L1(i.e. for chemical bondWithIt is connected directly), C1-C12Linear chain or branched chain alkylidene, C5-C30
Arlydene or C5-C30Heteroarylidene；
Condition is to work as L1When not being chemical bond, L1Upper arbitrary hydrogen atom is optional substituted or non-substituted；
Wherein, work as L1There are when substituent group, the substituent group can be halogen (F, Cl, Br or I), hydroxyl, amino, nitre
Base, itrile group, sulfydryl, C1-C5Alkoxy, C1-C5Alkyl；It can be with when the quantity of substituent group is greater than 1, between different substituent groups
It is independently identical or different.
Preferably, L1For chemical bond, C1-C6Linear chain or branched chain alkylidene (such as methylene, ethylidene, propylidene, Asia
Butyl, pentylidene, octamethylene etc.) or C5-C12Arlydene (such as phenylene, naphthylene etc.)；
Condition is to work as L1When not being chemical bond, L1Upper arbitrary hydrogen atom is optional substituted or non-substituted；
Wherein, work as L1There are when substituent group, the substituent group can be halogen (F, Cl, Br or I), hydroxyl, amino, nitre
Base, itrile group, sulfydryl, C1-C5Alkoxy, C1-C5Alkyl；It can be with when the quantity of substituent group is greater than 1, between different substituent groups
It is independently identical or different.
In a currently preferred embodiment, L1For chemical bond, l, m are independently whole more than or equal to 0
Number, and l+m >=1.
In currently preferred some embodiments, L1For C1-C6Straight-chain alkyl-sub (more preferably non-substituted branch
Alkylidene), l, m are independently the integer more than or equal to 1.
In a currently preferred embodiment, L1For C5-C12Arlydene (more preferably non-substituted arlydene),
L, m is independently the integer more than or equal to 1.
In preferred some embodiments of the invention, formula (I) compound are as follows:
OrOne or more of.
(c) anti-dropping agent:
Anti-dropping agent used includes: TF-1645, PA5933, PA5935, MM-5935, TF9207, PA5955 in the present invention
(3MDyneon company, the U.S.), DymgardTMFRS-5501, FA500H (big King Company), one or more of FC4530.
Further, in melt-drip resistant inflaming retarding polyester composite of the present invention, each raw material component is according to mass fraction meter, dosage
It is as follows:
50~100 parts of PET resin, such as can be, but be not limited to 55,60,65,70,75,80,85,90 or 95 parts
Deng；1~50 part of fire retardant of bridge chain DOPO derivative species, such as can be, but be not limited to 3,5,10,15,20,25,30,35,40,
Or 45 parts etc.；0.05~3 part of anti-dropping agent, such as can be, but be not limited to 0.1,0.5,0.8,1,1.2,1.5,1.8,2,
2.2,2.5 or 2.8 parts etc..
Preferably, in melt-drip resistant inflaming retarding polyester composite of the present invention, each raw material component is according to mass fraction meter, and dosage is such as
Under: 55~95 parts of PET resin, 5~30 parts of fire retardant, 0.1~2 part of anti-dropping agent of bridge chain DOPO derivative species.
Further, the present invention as above arbitrarily be formulated and material quality part array at melt-drip resistant inflaming retarding polyester composite
Following method is referred to be prepared:
Firstly, each raw material is carried out pre-dried, comprising: by PET resin under the conditions of 80~95 DEG C, dry 12~
36h (preferably under the conditions of 85~90 DEG C, drying is for 24 hours)；
The predrying of bridge chain DOPO derivative species fire retardant includes: by bridge chain DOPO derivative species fire retardant at 80~95 DEG C
Under the conditions of, dry 1~6h (preferably under the conditions of 85~90 DEG C, dry 2~5h)；
The predrying of anti-dropping agent include: by bridge chain DOPO derivative species fire retardant under the conditions of 80~95 DEG C, dry 1~
6h (preferably under the conditions of 85~90 DEG C, dry 2~5h).
Then, each raw material of formula ratio is added in extruder, extruder melting temperature be 200~350 DEG C (preferably
220~280 DEG C), under the conditions of the revolving speed of screw rod is 200~350r/min, the processing of melt blending extruding pelletization is carried out, is obtained anti-molten
Drip flame retardant polyester composite material.
By in the obtained melt-drip resistant inflaming retarding polyester composite of the present invention of method as above, since fire retardant can uniformly divide
It dissipates in PET matrix, and there is good compatibility with PET, so that composite material of the present invention is able to maintain PET itself
There is good mechanical performance, and fire retardant can also cooperate with the anti-dripping agent added on a small quantity, hence it is evident that improve the resistance of PET
Fire performance (vertical combustion grade is up to UL94V-0) and molten drop phenomenon.
Further, melt-drip resistant inflaming retarding polyester composite of the present invention is by the excellent properties that have, so can be into
One step has in the field of higher level flame retardant property, such as fibrous material/electronic device and/or the vehicles, and/or dress
Adorn construction material etc..
In the following examples and comparative examples, raw materials used PET resin is commercially available PT7450, and manufacturer is that Dupont is public
Department.
Embodiment 1
Melt-drip resistant inflaming retarding polyester composite described in the present embodiment the preparation method is as follows:
(1) raw material is weighed according to following parts by weight: 80 parts of PET resin, 8 parts of fire retardant of bridge chain DOPO derivative species, TF-
1645 0.2 part of anti-dropping agent.
The structural formula of fire retardant is as follows:
It is dried for 24 hours under the conditions of by PET resin at 85-90 DEG C；Fire retardant, anti-dropping agent are dry under the conditions of 85-90 DEG C
2-5h；
(2) PET resin, fire retardant and the anti-dropping agent after will be dry obtained in step (1) be equal in stirrer for mixing
It is even, obtain mixed resin；
(3) mixed resin melting extrusion obtained in step (2) is granulated, obtains the melt-drip resistant inflaming retarding polyester of embodiment 1
Composite material.
Wherein, it is 220 DEG C that the condition of melting extrusion, which includes: area's temperature, and two area's temperature are 240 DEG C, and three area's temperature are 250
DEG C, four area's temperature are 260 DEG C, and five area's temperature are 270 DEG C；Screw speed is 200-350rpm/min.
Embodiment 2
(1) raw material is weighed according to following parts by weight: 80 parts of PET resin, 8 parts of fire retardant of bridge chain DOPO derivative species,
0.2 part of PA5935 anti-dropping agent.
The structural formula of fire retardant is as follows:
PET resin is dried for 24 hours under the conditions of 85-90 DEG C；Fire retardant, anti-dropping agent dry 2- under the conditions of 85-90 DEG C
5h。
(2) PET resin, fire retardant and the anti-dropping agent after will be dry obtained in step (1) be equal in stirrer for mixing
It is even, obtain mixed resin；
(3) mixed resin melting extrusion obtained in step (2) is granulated, obtains the melt-drip resistant inflaming retarding polyester of embodiment 2
Composite material.
The condition of melting extrusion include: area's temperature be 220 DEG C, two area's temperature be 240 DEG C, three area's temperature be 250 DEG C, four
Area's temperature is 260 DEG C, and five area's temperature are 270 DEG C；Screw speed is 200-350rpm/min.
Embodiment 3
(1) raw material is weighed according to following parts by weight: 80 parts of PET resin, 8 parts of fire retardant of bridge chain DOPO derivative species, TF-
1645 0.1 part of anti-dropping agent, 0.1 part of FC4530 anti-dropping agent.
The structural formula of fire retardant is as follows:
PET resin is dried for 24 hours under the conditions of 85-90 DEG C；Fire retardant, anti-dropping agent predrying are under the conditions of 85-90 DEG C
Dry 2-5h.
(2) PET resin, fire retardant and the anti-dropping agent after will be dry obtained in step (1) be equal in stirrer for mixing
It is even, obtain mixed resin.
(3) mixed resin melting extrusion obtained in step (2) is granulated, obtains the melt-drip resistant inflaming retarding polyester of embodiment 3
Composite material.
The condition of melting extrusion include: area's temperature be 220 DEG C, two area's temperature be 240 DEG C, three area's temperature be 250 DEG C, four
Area's temperature is 260 DEG C, and five area's temperature are 270 DEG C；Screw speed is 200-350rpm/min.
Embodiment 4
(1) raw material is weighed according to following parts by weight: 80 parts of PET resin, two kinds of bridge chain DOPO derivative species fire retardants each 4
Part, DymgardTM0.2 part of FRS-5501 anti-dropping agent.
The structural formula of the fire retardant is as follows:
PET resin is dried for 24 hours under the conditions of 85-90 DEG C；Fire retardant, anti-dropping agent dry 2-5h under the conditions of 85-90 DEG C.
(2) PET resin, fire retardant and the anti-dropping agent after will be dry obtained in step (1) be equal in stirrer for mixing
It is even, obtain mixed resin；
(3) mixed resin melting extrusion obtained in step (2) is granulated, obtains the melt-drip resistant inflaming retarding polyester of embodiment 4
Composite material.
The condition of melting extrusion include: area's temperature be 220 DEG C, two area's temperature be 240 DEG C, three area's temperature be 250 DEG C, four
Area's temperature is 260 DEG C, and five area's temperature are 270 DEG C；Screw speed is 200-350rpm/min.
Comparative example 1
The preparation method of the composite material of 1 reference implementation example 1 of comparative example, difference are that comparative example 1 uses pure PET resin,
Fire retardant or anti-dripping agent are not added.
Comparative example 2
(1) raw material is weighed according to following parts by weight: 80 parts of PET resin, 8 parts of fire retardant of bridge chain DOPO derivative species, institute
The structural formula for stating fire retardant is as follows:
PET resin is dried for 24 hours under the conditions of 85-90 DEG C；Fire retardant dry 2-5h under the conditions of 85-90 DEG C.
(2) PET resin and fire retardant after will be dry obtained in step (1) be uniform in stirrer for mixing, are mixed
Close base-material；
(3) mixed resin melting extrusion obtained in step (2) is granulated, obtains the melt-drip resistant inflaming retarding polyester of comparative example 2
Composite material.
The condition of melting extrusion include: area's temperature be 220 DEG C, two area's temperature be 240 DEG C, three area's temperature be 250 DEG C, four
Area's temperature is 260 DEG C, and five area's temperature are 270 DEG C；Screw speed is 200-350rpm/min.
Experimental example 1
The flame retardant property of the material of embodiment 1-4 and comparative example 1-2 and mechanical property performance are tested respectively,
The test method of middle flame retardant property is carried out with reference to ASTM UL 94-2006 standard and ASTM D 2863-97 standard, mechanical property
Test method is carried out with reference to GB-1040.1-2006 standard, and test result is as follows shown in table 1.
The flame retardant property and mechanical experimental results of 1 different materials of table
* non-antiflaming rank is indicated
The data as shown in upper table table are it is found that DOPO derivative flame retardant in 1-4 of the embodiment of the present invention containing phenyl ring, association
Effect adds a small amount of anti-dripping agent, can inhibit the high temperature molten drop of PET existing while guaranteeing the flame retardant property of PET composite material
As.
Meanwhile it can compared with the mechanical performance of comparative example 1 by the mechanical performance of embodiment 1-4,2 composite material of comparative example
Know, the DOPO derivative flame retardant used containing phenyl ring has good compatibility with substrate PET in the present invention, will not influence PET
The original mechanical performance of material.
It further, can compared with the fire-retardant and anti-dripping melt performance of Comparative Examples 1 and 2 material by embodiment 1-4 composite material
Know, although fire retardant, which is used only, can also improve the flame retardant property and molten drop phenomenon of PET, however, if by fire retardant and on a small quantity
Anti-dripping agent be used in compounding, then be capable of it is more efficiently improve composite material flame retardant property and anti-dropping performance.
Although illustrate and describing the present invention with specific embodiment, it will be appreciated that without departing substantially from of the invention
Many other change and modification can be made in the case where spirit and scope.It is, therefore, intended that in the following claims
Including belonging to all such changes and modifications in the scope of the invention.
Claims (10)
1. a kind of melt-drip resistant inflaming retarding polyester composite, which is characterized in that the melt-drip resistant inflaming retarding polyester composite mainly by
The following raw material is made:
PET resin, bridge chain DOPO derivative species fire retardant and anti-dropping agent；
Wherein, the bridge chain DOPO derivative species fire retardant includes such as following formula (I) structural compounds:
Wherein, in formula (I), l, m are independently the integer more than or equal to 0；
Condition is that l, m are not 0 simultaneously；
L1For chemical bond, C1-C12Linear chain or branched chain alkylidene, C5-C30Arlydene or C5-C30Heteroarylidene；
Condition is to work as L1When not being chemical bond, L1Upper arbitrary hydrogen atom is optional substituted or non-substituted.
2. melt-drip resistant inflaming retarding polyester composite according to claim 1, which is characterized in that in formula (I), L1For chemical bond,
C1-C6Linear chain or branched chain alkylidene or C5-C12Arlydene；
Condition is to work as L1When not being chemical bond, L1Upper arbitrary hydrogen atom is optional substituted or non-substituted.
3. melt-drip resistant inflaming retarding polyester composite according to claim 1, which is characterized in that in parts by weight, respectively
Amounts of components is as follows:
50~100 parts of PET resin, 1~50 part of fire retardant, 0.05~3 part of anti-dropping agent of bridge chain DOPO derivative species.
4. melt-drip resistant inflaming retarding polyester composite according to claim 3, which is characterized in that in parts by weight, respectively
Amounts of components is as follows:
55~95 parts of PET resin, 5~30 parts of fire retardant, 0.1~2 part of anti-dropping agent of bridge chain DOPO derivative species.
5. the preparation method of melt-drip resistant inflaming retarding polyester composite of any of claims 1-4, which is characterized in that packet
It includes:
PET resin and bridge chain DOPO derivative species fire retardant, anti-dropping agent are subjected to melt blending processing after evenly mixing, obtained
Melt-drip resistant inflaming retarding polyester composite.
6. preparation method according to claim 5, which is characterized in that melt blending processing include using extruder into
The processing of row melt blending.
7. preparation method according to claim 6, which is characterized in that the temperature of extruder melting is 200~350 DEG C, spiral shell
The revolving speed of bar is 200~350r/min.
8. preparation method according to claim 5, which is characterized in that the preparation method further includes by PET resin, bridge chain
After DOPO derivative species fire retardant and anti-dropping agent carry out predrying, then the step of carrying out melt blending processing.
9. preparation method according to claim 8, which is characterized in that the predrying of PET resin includes: that PET resin exists
Under the conditions of 80~95 DEG C, dry 12~36h；
The predrying of bridge chain DOPO derivative species fire retardant includes: by bridge chain DOPO derivative species fire retardant in 80~95 DEG C of conditions
Under, dry 1~6h；
The predrying of anti-dropping agent includes: dry 1~6h by bridge chain DOPO derivative species fire retardant under the conditions of 80~95 DEG C.
10. melt-drip resistant inflaming retarding polyester composite of any of claims 1-4 is in fibrous material or electronic apparatus
Application；
And/or melt-drip resistant inflaming retarding polyester composite answering in communications and transportation of any of claims 1-4
With；
And/or melt-drip resistant inflaming retarding polyester composite of any of claims 1-4 is in decorative building material field
Using.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910124096.5A CN109777056B (en) | 2019-02-19 | 2019-02-19 | Anti-dripping flame-retardant polyester composite material and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910124096.5A CN109777056B (en) | 2019-02-19 | 2019-02-19 | Anti-dripping flame-retardant polyester composite material and preparation method and application thereof |
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| CN109777056A true CN109777056A (en) | 2019-05-21 |
| CN109777056B CN109777056B (en) | 2021-07-16 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5356250A (en) * | 1976-11-02 | 1978-05-22 | Toyobo Co Ltd | Polyeser composition |
| CN103703070A (en) * | 2011-07-28 | 2014-04-02 | 丸菱油化工业株式会社 | Flame retarder comprising condensed phosphonic acid ester and flame-retardant resin composition |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2126693A2 (en) * | 2006-12-29 | 2009-12-02 | Sandisk Corporation | Methods and apparatuses for launching a program application |
-
2019
- 2019-02-19 CN CN201910124096.5A patent/CN109777056B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5356250A (en) * | 1976-11-02 | 1978-05-22 | Toyobo Co Ltd | Polyeser composition |
| CN103703070A (en) * | 2011-07-28 | 2014-04-02 | 丸菱油化工业株式会社 | Flame retarder comprising condensed phosphonic acid ester and flame-retardant resin composition |
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| CN109777056B (en) | 2021-07-16 |
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