CN104231314A - Triazine triphenyl phosphinic acid isopropyl ester flame retardant composition and application method thereof - Google Patents

Triazine triphenyl phosphinic acid isopropyl ester flame retardant composition and application method thereof Download PDF

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Publication number
CN104231314A
CN104231314A CN201410507986.1A CN201410507986A CN104231314A CN 104231314 A CN104231314 A CN 104231314A CN 201410507986 A CN201410507986 A CN 201410507986A CN 104231314 A CN104231314 A CN 104231314A
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ttpi
flame retardant
pems
dopo
mpp
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CN201410507986.1A
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CN104231314B (en
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孙艳艳
俞春雷
王彦林
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Xiangcheng Institute of Suzhou University of Science and Technology
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Xiangcheng Institute of Suzhou University of Science and Technology
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Abstract

The invention relates to a triazine triphenyl phosphinic acid isopropyl 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 isopropyl ester (TTPI) at any proportion, wherein the weight part of the TTPI 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

Triazinyl triphenyl isopropyl phosphinate flame retardant composition and application method thereof
Technical field
The present invention relates to a kind of Triazinyl triphenyl isopropyl phosphinate flame retardant composition and application method thereof, this flame retardant composition can be used as the fire retardant of the materials such as polyester PET, polyester PBT, urethane, polypropylene, epoxy resin.
Background technology
General organophosphorous fire retardant mostly is liquid, have that molecular weight is little, polarity be large, poor heat resistance, volatility are large, the amount of being fuming is large, with poor compatibility, little, the easy migration of range of application of material, the shortcoming such as phosphorus content is low, flame retardant properties is poor.Therefore market is badly in need of exploitation high comprehensive performance, the organic phosphine fire retardant of above-mentioned shortcoming can be overcome.Worked in coordination with by ignition-proof elements many in structure or many fire retardants composite be improve the effective way of flame-retarded efficiency, be wherein one of important research direction finding excellent halogen-free flame retardants to the research of phosphorus, nitrogen synergistic fire retardant.Due to the nitrogenous organic phosphine compound based on triazine ring derivatives there is Halogen, low toxicity, decomposition temperature is high, fire retardant is not separated out, can give the material better feature such as fire-retardant and machining property, fire retardant is composite also can produce good synergistic function by itself and other.Therefore, the research of this based flame retardant more and more comes into one's own.
The invention discloses a kind of Triazinyl triphenyl isopropyl phosphinate flame retardant composition and application method thereof, Triazinyl triphenyl isopropyl phosphinate in this flame retardant composition contains C-P key and stable fragrant phosphine key, Stability Analysis of Structures, also containing symmetrical virtue-large conjugated system of phosphine-nitrogen and polyester structure, itself and material have good consistency.Synergistic function is produced by the different structure in complex composition, multiple ignition-proof element; when burning; ignition-proof element phosphorus is wherein easy to be formed fine and close and uniform polyphosphoric acid protective membrane; element silicon promotes to form fine and close silicon-charcoal protective layer; nitrogen element can play the multiple fire retardations such as expansion, heat insulation anoxybiotic, cooling, shows excellent flame-retarded efficiency.Flame retardant composition cooperative flame retardant is effective, and have good consistency with macromolecular material, stability is high, is adapted to the high temperature process of material, does not reduce the physical strength of material.And this flame retardant composition preparation method is simple, can reduce costs, have good application prospect.
Summary of the invention
An object of the present invention is to propose a kind of Triazinyl triphenyl isopropyl phosphinate flame retardant composition.This flame retardant composition cooperative flame retardant usefulness is high, and Halogen, meets environmental requirement, can overcome the deficiencies in the prior art, can be widely used as the fire retardant of the materials such as polyester, urethane, polypropylene, epoxy resin, have good application and development prospect.
Another object of the present invention is to propose the application method of a kind of Triazinyl triphenyl isopropyl phosphinate flame retardant composition in the materials such as polyester PET, polyester PBT, urethane, polypropylene, epoxy resin.
The object of the invention is to be achieved through the following technical solutions:
A kind of Triazinyl triphenyl isopropyl phosphinate flame retardant composition, it is by melamine cyanurate (being called for short MCA), melamine polyphosphate (being called for short MPP), 9, mix in-10-phospho hetero phenanthrene-10-oxide compound (be called for short DOPO), pentaerythritol methylsilicate (being called for short PEMS) any two kinds, three kinds or four kinds of, Homogeneous phase mixing composite with arbitrary proportion with Triazinyl triphenyl isopropyl phosphinate (being called for short TTPI) of 10-dihydro-9-oxy obtain, and the weight fraction of TTPI is greater than zero.But consider reduction and the flame retardant properties of price, the compound proportion that recommendation tables 1 is stated.Table 1 is the per-cent that each component accounts for flame retardant composition gross weight.
The each formulation ratio table of table 1 flame retardant composition
Wherein the structure of TTPI 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 method of flame retardant composition of the present invention described above, to be applied as example in polyester PET or PBT, is characterized in that, the method is:
In polyester PET or PBT, add the flame retardant composition of formula 1, formula 2, formula 3, formula 4, formula 5, formula 6 or formula 7 respectively, mix, injection moulding or extrude under melt temperature.
Compared with prior art, beneficial effect of the present invention is:
1. the TTPI in flame retardant composition of the present invention is the many phosphorus of many aromatic rings macromole, many nitrogen, polyester compound, has good consistency with macromolecular material, is easy to dispersion, does not separate out, do not reduce the physical strength of material.
2. fire retardant of the present invention does not conform to halogen, meets environmental requirement, has good application and development prospect.
3. flame retardant composition provided by the invention, containing phosphorus, nitrogen or element silicon, can produce synergistic fire retardation, has good flame-retarded efficiency to polyester PET, PBT.
4. the preparation method of flame retardant composition provided by the invention is simple, and facility investment is few, and production cost is low, and application is convenient.
Embodiment
Provide embodiment below so that the present invention is further illustrated; but be pointed out that following examples can not be interpreted as limiting the scope of the invention, some nonessential improvement that person skilled in the art's foregoing according to the present invention of this area is made the present invention and adjustment still belong to protection scope of the present invention.
Embodiment 1 adds TTPI, MCA and DOPO of different ratios in polyester PET, stirs, and extrudes with XJ-01 type forcing machine the batten that diameter is about 3mm under melt temperature, surveys its limiting oxygen index(LOI), the results are shown in Table 2 with HC900-2 type oxygen index measurer.
Table 2 TTPI and MCA and DOPO is composite to the fire-retardant data of PET
Embodiment 2 adds TTPI, MCA and PEMS of different ratios in polyester PET, stirs, and extrudes with XJ-01 type forcing machine the batten that diameter is about 3mm under melt temperature, surveys its limiting oxygen index(LOI), the results are shown in Table 3 with HC900-2 type oxygen index measurer.
Table 3 TTPI and MCA and PEMS is composite to the fire-retardant data of PET
Embodiment 3 adds TTPI, MPP and DOPO of different ratios in polyester PET, stirs, and extrudes with XJ-01 type forcing machine the batten that diameter is about 3mm under melt temperature, surveys its limiting oxygen index(LOI), the results are shown in Table 4 with HC900-2 type oxygen index measurer.
Table 4 TTPI and MPP and DOPO is composite to the fire-retardant data of PET
Embodiment 4 adds TTPI, MPP and PEMS of different ratios in polyester PET, stirs, and extrudes with XJ-01 type forcing machine the batten that diameter is about 3mm under melt temperature, surveys its limiting oxygen index(LOI), the results are shown in Table 5 with HC900-2 type oxygen index measurer.
Table 5 TTPI and MPP and PEMS is composite to the fire-retardant data of PET
Embodiment 5 adds TTPI, MCA, DOPO and PEMS of different ratios in polyester PET, stir, under melt temperature, extrude with XJ-01 type forcing machine the batten that diameter is about 3mm, survey its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 6.
Table 6 TTPI and MCA, DOPO and PEMS are composite to the fire-retardant data of PET
Embodiment 6 adds TTPI, MPP, DOPO and PEMS of different ratios in polyester PET, stir, under melt temperature, extrude with XJ-01 type forcing machine the batten that diameter is about 3mm, survey its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 7.
Table 7 TTPI and MPP, DOPO and PEMS are composite to the fire-retardant data of PET
Embodiment 7 adds TTPI, MCA, MPP, DOPO and PEMS of different ratios in polyester PET, stir, under melt temperature, extrude with XJ-01 type forcing machine the batten that diameter is about 3mm, survey its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 8.
Table 8 TTPI and MCA, MPP, DOPO and PEMS are composite to the fire-retardant data of PET
Embodiment 8 adds TTPI, MCA and DOPO of different ratios in polyester PBT, stirs, and extrudes with XJ-01 type forcing machine the batten that diameter is about 3mm under melt temperature, surveys its limiting oxygen index(LOI), the results are shown in Table 9 with HC900-2 type oxygen index measurer.
Table 9 TTPI and MCA and DOPO is composite to the fire-retardant data of PBT
Embodiment 9 adds TTPI, MCA and PEMS of different ratios in polyester PBT, stirs, and extrudes with XJ-01 type forcing machine the batten that diameter is about 3mm under melt temperature, surveys its limiting oxygen index(LOI), the results are shown in Table 10 with HC900-2 type oxygen index measurer.
Table 10 TTPI and MCA and PEMS is composite to the fire-retardant data of PBT
Embodiment 10 adds TTPI, MPP and DOPO of different ratios in polyester PBT, stirs, and extrudes with XJ-01 type forcing machine the batten that diameter is about 3mm under melt temperature, surveys its limiting oxygen index(LOI), the results are shown in Table 11 with HC900-2 type oxygen index measurer.
Table 11 TTPI and MPP and DOPO is composite to the fire-retardant data of PBT
Embodiment 11 adds TTPI, MPP and PEMS of different ratios in polyester PBT, stirs, and extrudes with XJ-01 type forcing machine the batten that diameter is about 3mm under melt temperature, surveys its limiting oxygen index(LOI), the results are shown in Table 12 with HC900-2 type oxygen index measurer.
Table 12 TTPI and MPP and PEMS is composite to the fire-retardant data of PBT
Embodiment 12 adds TTPI, MCA, DOPO and PEMS of different ratios in polyester PBT, stir, under melt temperature, extrude with XJ-01 type forcing machine the batten that diameter is about 3mm, survey its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 13.
Table 13 TTPI and MCA, DOPO and PEMS are composite to the fire-retardant data of PBT
Embodiment 13 adds TTPI, MPP, DOPO and PEMS of different ratios in polyester PBT, stir, under melt temperature, extrude with XJ-01 type forcing machine the batten that diameter is about 3mm, survey its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 14.
Table 14 TTPI and MPP, DOPO and PEMS are composite to the fire-retardant data of PBT
Embodiment 14 adds TTPI, MCA, MPP, DOPO and PEMS of different ratios in polyester PBT, stir, under melt temperature, extrude with XJ-01 type forcing machine the batten that diameter is about 3mm, survey its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 15.
Table 15 TTPI and MCA, MPP, DOPO and PEMS are composite to the fire-retardant data of PBT

Claims (2)

1. a Triazinyl triphenyl isopropyl phosphinate flame retardant composition, it is characterized in that, this flame retardant composition is by melamine cyanurate (being called for short MCA), melamine polyphosphate (being called for short MPP), 9,10-dihydro-9-oxy mix in-10-phospho hetero phenanthrene-10-oxide compound (be called for short DOPO) and pentaerythritol methylsilicate (being called for short PEMS) any two kinds, three kinds or four kinds composite with arbitrary proportion with Triazinyl triphenyl isopropyl phosphinate (being called for short TTPI), Homogeneous phase mixing obtained, and the weight fraction of TTPI is greater than zero
Wherein the structure of TTPI 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:
2. a kind of application method of Triazinyl triphenyl isopropyl phosphinate flame retardant composition is according to claim 1: in polyester PET or PBT, add TTPI, MCA and DOPO of different ratios or TTPI, MCA and PEMS or TTPI, MPP and DOPO or TTPI, MPP and PEMS or TTPI, MCA, DOPO and PEMS or TTPI, MPP, DOPO and PEMS or TTPI, MCA, MPP, DOPO and PEMS, mix, injection moulding or extrude under melt temperature.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107286342A (en) * 2017-08-07 2017-10-24 顺德职业技术学院 " phosphorus silicon nitrogen " oligomer formula expansion type flame retardant and its synthetic method containing triazine ring

Citations (2)

* Cited by examiner, † Cited by third party
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107286342A (en) * 2017-08-07 2017-10-24 顺德职业技术学院 " phosphorus silicon nitrogen " oligomer formula expansion type flame retardant and its synthetic method containing triazine ring

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