CN104231315B - Triazine triphenyl phosphinic acid tert-butyl ester flame retardant composition and application method thereof - Google Patents
Triazine triphenyl phosphinic acid tert-butyl ester flame retardant composition and application method thereof Download PDFInfo
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- CN104231315B CN104231315B CN201410507990.8A CN201410507990A CN104231315B CN 104231315 B CN104231315 B CN 104231315B CN 201410507990 A CN201410507990 A CN 201410507990A CN 104231315 B CN104231315 B CN 104231315B
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Abstract
The invention relates to a triazine triphenyl phosphinic acid tert-butyl ester flame retardant composition and an application method thereof. The flame retardant composition is prepared by compounding and uniformly mixing any two, three or four of melamine cyanurate (MCA), melamine pyrophosphate (MPP), 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and pentaerythritol methyl silicate (PEMS) with triazine triphenyl phosphinic acid tert-butyl ester (TTPT) at any proportion, wherein the weight part of the TTPT is greater than zero. The flame retardant composition provided by the invention has the advantages of multielement synergic effect, good flame retardancy, good compatibility with materials, low cost, zero halogen, environmental protection and the like, can be used as a flame retardant for polyester PET, polyester PBT, polyurethane, polypropylene, epoxy resin and other materials, and has excellent application and popularization prospects.
Description
Technical field
The present invention relates to a kind of triazine triphenyl phosphinic acid tert-butyl ester fire retardant combination and application process, this fire retardant
Compositions can be used as the fire retardant of the materials such as polyester PET, polyester PBT, polyurethane, polypropylene, epoxy resin.
Background technology
Along with progress and the extensive application of macromolecular material of science and technology, fire retardant industry has obtained development quickly.
Improving constantly along with people's living standard simultaneously, safety consciousness constantly strengthens, and the flame retardant regulation of requirements at the higher level is constantly put into effect, halogen
The application of flame retardant is restricted in many aspects, and the research and development to halogen-free flame retardants have the strongest urgency.Ability
Field technique personnel think that phosphorus-nitrogen containing flame retardant is the main force realizing non-halogen fire retardant.Research finds that multielement synergetic is organic
Phosphine fire retardant advantage is a lot, can give that material is the most fire-retardant and machining property.Thus design intramolecular multielement is worked in coordination with
Or realize the collaborative important means having become the research of current flame-retarded technology of multielement by compounding.Wherein spread out with stable triazine ring
Biology is carrier structure phosphorus nitrogen or the molecular structure of more ignition-proof element, can bring highly effective flame-retardant and become charcoal effect, to carrying
High flame resistance has obvious synergistic function.Above-mentioned fire retardant and other fire retardant be compounding also can produce excellent fire-retardant
Effect.
The invention discloses a kind of triazine triphenyl phosphinic acid tert-butyl ester fire retardant combination and application process thereof, this is fire-retardant
Triazine triphenyl phosphinic acid tert-butyl ester in agent compositions contains C-P key and stable fragrant phosphine key, and Stability Analysis of Structures, possibly together with symmetry
Virtue-big conjugated system of phosphine-nitrogen and many ester structures, it has the preferable compatibility with material.By the difference in complex composition
Structure, multiple ignition-proof element produce synergistic function, and when burning, ignition-proof element phosphorus therein is readily formed densification and equal
Even polyphosphoric acid protecting film, element silicon promotes to form fine and close silicon-charcoal protective layer, and nitrogen element can play expansion, heat insulation anoxybiotic, fall
The multiple fire retardations such as temperature, show excellent flame-retarded efficiency.Fire retardant combination cooperative flame retardant is effective, with macromolecular material
Having the good compatibility, stability is high, is adapted to the high temperature process of material, does not reduce the mechanical strength of material.And this is fire-retardant
Agent preparation method of composition is simple, can reduce cost, have good application prospect.
Summary of the invention
An object of the present invention is to propose a kind of triazine triphenyl phosphinic acid tert-butyl ester fire retardant combination.This is fire-retardant
Agent compositions cooperative flame retardant usefulness is high, and Halogen meets environmental requirement, can overcome the deficiencies in the prior art, be widely used as polyester,
The fire retardant of the materials such as polyurethane, polypropylene, epoxy resin, has good application and development prospect.
Another object of the present invention is to propose a kind of triazine triphenyl phosphinic acid tert-butyl ester fire retardant combination at polyester
Application process in the materials such as PET, polyester PBT, polyurethane, polypropylene, epoxy resin.
It is an object of the invention to be achieved through the following technical solutions:
A kind of triazine triphenyl phosphinic acid tert-butyl ester fire retardant combination, it is (to be called for short by melamine cyanurate
MCA), melamine polyphosphate (being called for short MPP), 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (are called for short
DOPO), any two kinds, three kinds or four kinds in pentaerythritol methylsilicate (being called for short PEMS) and triazine triphenyl phosphinic acid uncle
Butyl ester (being called for short TTPT) compounds with arbitrary proportion, is uniformly mixed to prepare, and the weight fraction of TTPT is more than zero.But consider price
Reduce and fire resistance, it is recommended that the compound proportion that table 1 is stated.Table 1 is the percentage that each component accounts for fire retardant combination gross weight
Ratio.
Table 1 fire retardant combination each formulation ratio table
Wherein the structure of TTPT is shown below:
The structure of MCA is shown below:
The structure of MPP is shown below:
The structure of DOPO is shown below:
The structure of PEMS is shown below:
The application process of fire retardant combination of the present invention as mentioned above, as a example by application in polyester PET or PBT, it is special
Levying and be, the method is:
Formula 1, formula 2, formula 3, formula 4, formula 5, formula 6 or formula 7 it is separately added in polyester PET or PBT
Fire retardant combination, mix homogeneously, it is molded under melt temperature or extrudes.
Compared with prior art, the beneficial effects of the present invention is:
TTPT in fire retardant combination the most of the present invention is the many phosphorus of many aromatic rings macromole, many nitrogen, many ester compounds, with high score
Sub-material has the good compatibility, it is easy to dispersion, does not separates out, does not reduce the mechanical strength of material.
2. the fire retardant of the present invention does not contains halogen, meets environmental requirement, has good application and development prospect.
3. the fire retardant combination that the present invention provides, containing phosphorus, nitrogen or element silicon, can produce synergistic fire retardation, to poly-
Ester PET, PBT have good flame-retarded efficiency.
4. the preparation method of the fire retardant combination that the present invention provides is simple, and equipment investment is few, and production cost is low, application side
Just.
Detailed description of the invention
Embodiment it is given below so that the present invention is further illustrated, but is pointed out that following example are not understood that
For limiting the scope of the invention, the present invention is made by the person skilled in the art of this area according to the foregoing of the present invention
Some nonessential improvement and adjustment still fall within protection scope of the present invention.
Embodiment 1 adds TTPT, MCA and DOPO of different proportion in polyester PET, stirs, and squeezes by XJ-01 type
Go out machine under melt temperature, extrude the batten of diameter about 3mm, survey its limited oxygen index with HC900-2 type oxygen index measurer, knot
Fruit is shown in Table 2.
Table 2 TTPT Yu MCA and DOPO compounds data fire-retardant to PET
Embodiment 2 adds TTPT, MCA and PEMS of different proportion in polyester PET, stirs, and squeezes by XJ-01 type
Go out machine under melt temperature, extrude the batten of diameter about 3mm, survey its limited oxygen index with HC900-2 type oxygen index measurer, knot
Fruit is shown in Table 3.
Table 3 TTPT Yu MCA and PEMS compounds data fire-retardant to PET
Embodiment 3 adds TTPT, MPP and DOPO of different proportion in polyester PET, stirs, and squeezes by XJ-01 type
Go out machine under melt temperature, extrude the batten of diameter about 3mm, survey its limited oxygen index with HC900-2 type oxygen index measurer, knot
Fruit is shown in Table 4.
Table 4 TTPT Yu MPP and DOPO compounds data fire-retardant to PET
Embodiment 4 adds TTPT, MPP and PEMS of different proportion in polyester PET, stirs, and squeezes by XJ-01 type
Go out machine under melt temperature, extrude the batten of diameter about 3mm, survey its limited oxygen index with HC900-2 type oxygen index measurer, knot
Fruit is shown in Table 5.
Table 5 TTPT Yu MPP and PEMS compounds data fire-retardant to PET
Embodiment 5 adds TTPT, MCA, DOPO and PEMS of different proportion in polyester PET, stirs, and uses XJ-
The batten of diameter about 3mm extruded under melt temperature by 01 type extruder, surveys its limit oxygen with HC900-2 type oxygen index measurer and refers to
Number, the results are shown in Table 6.
Table 6 TTPT Yu MCA, DOPO and PEMS compound data fire-retardant to PET
Embodiment 6 adds TTPT, MPP, DOPO and PEMS of different proportion in polyester PET, stirs, and uses XJ-
The batten of diameter about 3mm extruded under melt temperature by 01 type extruder, surveys its limit oxygen with HC900-2 type oxygen index measurer and refers to
Number, the results are shown in Table 7.
Table 7 TTPT Yu MPP, DOPO and PEMS compound data fire-retardant to PET
Embodiment 7 adds TTPT, MCA, MPP, DOPO and PEMS of different proportion in polyester PET, stirs, and uses
The batten of diameter about 3mm extruded under melt temperature by XJ-01 type extruder, surveys its limit with HC900-2 type oxygen index measurer
Oxygen index (OI), the results are shown in Table 8.
Table 8 TTPT Yu MCA, the compounding data fire-retardant to PET of MPP, DOPO and PEMS
Embodiment 8 adds TTPT, MCA and DOPO of different proportion in polyester PBT, stirs, and squeezes by XJ-01 type
Go out machine under melt temperature, extrude the batten of diameter about 3mm, survey its limited oxygen index with HC900-2 type oxygen index measurer, knot
Fruit is shown in Table 9.
Table 9 TTPT Yu MCA and DOPO compounds data fire-retardant to PBT
Embodiment 9 adds TTPT, MCA and PEMS of different proportion in polyester PBT, stirs, and squeezes by XJ-01 type
Go out machine under melt temperature, extrude the batten of diameter about 3mm, survey its limited oxygen index with HC900-2 type oxygen index measurer, knot
Fruit is shown in Table 10.
Table 10 TTPT Yu MCA and PEMS compounds data fire-retardant to PBT
Embodiment 10 adds TTPT, MPP and DOPO of different proportion in polyester PBT, stirs, and uses XJ-01 type
The batten of diameter about 3mm extruded under melt temperature by extruder, surveys its limited oxygen index with HC900-2 type oxygen index measurer,
The results are shown in Table 11.
Table 11 TTPT Yu MPP and DOPO compounds data fire-retardant to PBT
Embodiment 11 adds TTPT, MPP and PEMS of different proportion in polyester PBT, stirs, and uses XJ-01 type
The batten of diameter about 3mm extruded under melt temperature by extruder, surveys its limited oxygen index with HC900-2 type oxygen index measurer,
The results are shown in Table 12.
Table 12 TTPT Yu MPP and PEMS compounds data fire-retardant to PBT
Embodiment 12 adds TTPT, MCA, DOPO and PEMS of different proportion in polyester PBT, stirs, uses XJ-
The batten of diameter about 3mm extruded under melt temperature by 01 type extruder, surveys its limit oxygen with HC900-2 type oxygen index measurer and refers to
Number, the results are shown in Table 13.
Table 13 TTPT Yu MCA, DOPO and PEMS compound data fire-retardant to PBT
Embodiment 13 adds TTPT, MPP, DOPO and PEMS of different proportion in polyester PBT, stirs, uses XJ-
The batten of diameter about 3mm extruded under melt temperature by 01 type extruder, surveys its limit oxygen with HC900-2 type oxygen index measurer and refers to
Number, the results are shown in Table 14.
Table 14 TTPT Yu MPP, DOPO and PEMS compound data fire-retardant to PBT
Embodiment 14 adds TTPT, MCA, MPP, DOPO and PEMS of different proportion in polyester PBT, stirs,
Under melt temperature, extrude the batten of diameter about 3mm with XJ-01 type extruder, survey its pole with HC900-2 type oxygen index measurer
Limited oxygen index, the results are shown in Table 15.
Table 15 TTPT Yu MCA, the compounding data fire-retardant to PBT of MPP, DOPO and PEMS
Claims (2)
1. a triazine triphenyl phosphinic acid tert-butyl ester fire retardant combination, it is characterised in that this fire retardant combination is by three
Poly cyanamid cyanurate (be called for short MCA), melamine polyphosphate (being called for short MPP), 9,10-dihydro-9-oxy miscellaneous-10-phospho hetero phenanthrene-
Any two kinds, three kinds or four kinds and three in 10-oxide (being called for short DOPO) and pentaerythritol methylsilicate (being called for short PEMS)
Piperazine triphenyl phosphinic acid tert-butyl ester (being called for short TTPT) compounds with arbitrary proportion, is uniformly mixed to prepare, and the weight fraction of TTPT is big
In zero, MPP Yu MCA discord TTPT is re-dubbed three components compositions,
Wherein the structure of TTPT is shown below:
The structure of MCA is shown below:
The structure of MPP is shown below:
The structure of DOPO is shown below:
The structure of PEMS is shown below:
A kind of application process of triazine triphenyl phosphinic acid tert-butyl ester fire retardant combination, feature
Be: add in polyester PET or PBT different proportion TTPT, MCA and DOPO or add different proportion TTPT, MCA and
PEMS or add different proportion TTPT, MPP and DOP0 add different proportion TTPT, MPP and PEMS or add the most on year-on-year basis
TTPT, MCA, DOPO and PEMS of example or add TTPT, MPP, DOPO and PEMS of different proportion or add different proportion
TTPT, MCA, MPP, DOPO and PEMS, mix homogeneously, it is molded under melt temperature or extrudes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410507990.8A CN104231315B (en) | 2014-09-26 | 2014-09-26 | Triazine triphenyl phosphinic acid tert-butyl ester flame retardant composition and application method thereof |
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| CN201410507990.8A CN104231315B (en) | 2014-09-26 | 2014-09-26 | Triazine triphenyl phosphinic acid tert-butyl ester flame retardant composition and application method thereof |
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| CN104231315B true CN104231315B (en) | 2017-01-11 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101260202A (en) * | 2008-04-18 | 2008-09-10 | 公安部四川消防研究所 | Halogen-free expansion type fire retardant and flame-proof polypropylene material |
| CN103254235A (en) * | 2013-06-05 | 2013-08-21 | 苏州科技学院 | Butyl triazinyl triphenyl hypophosphite compound and preparation method thereof |
-
2014
- 2014-09-26 CN CN201410507990.8A patent/CN104231315B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101260202A (en) * | 2008-04-18 | 2008-09-10 | 公安部四川消防研究所 | Halogen-free expansion type fire retardant and flame-proof polypropylene material |
| CN103254235A (en) * | 2013-06-05 | 2013-08-21 | 苏州科技学院 | Butyl triazinyl triphenyl hypophosphite compound and preparation method thereof |
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