CN104231316A - Triazine triphenyl phosphinic acid sec-butyl ester flame retardant composition and application method thereof - Google Patents
Triazine triphenyl phosphinic acid sec-butyl ester flame retardant composition and application method thereof Download PDFInfo
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- CN104231316A CN104231316A CN201410508022.9A CN201410508022A CN104231316A CN 104231316 A CN104231316 A CN 104231316A CN 201410508022 A CN201410508022 A CN 201410508022A CN 104231316 A CN104231316 A CN 104231316A
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- 0 CC(*)P([N+](C)(c1nc(N)nc(N)n1)[O-])(OC)=O Chemical compound CC(*)P([N+](C)(c1nc(N)nc(N)n1)[O-])(OC)=O 0.000 description 1
Abstract
The invention relates to a triazine triphenyl phosphinic acid sec-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 sec-butyl ester (TTPS) at any proportion, wherein the weight part of the TTPS 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 the secondary butyl ester flame retardant composition of a kind of triazine triphenyl phospho acid 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
Along with improving constantly of people's living standard, macromolecular material is widely used, but causes fire frequently to occur due to its inflammable characteristic, causes serious threat, facilitate the fast development of fire retardant industry to the security of the lives and property of people.And along with the enhancing of people's safety and environmental protection consciousness, the continuous appearance of flame retardant regulation, the application of halogenated flame retardant is restricted in many aspects, has very strong urgency to the research and development of halogen-free flame retardants.Current phosphorus-nitrogen containing flame retardant is the main products realizing non-halogen fire retardant.Research finds that multielement synergetic organic phosphine fire retardant can give material better fire-retardant and machining property.Thus design multielement in molecule work in coordination with or work in coordination with by the composite multielement that realizes the important directions becoming the research of current flame-retarded technology.Wherein formed the molecular structure of phosphorus nitrogen or more ignition-proof element with stable triazine ring derivatives for carrier design, highly effective flame-retardant can be brought and become charcoal effect, to raising flame retardant properties, be there is obvious synergistic function.Above-mentioned fire retardant and other fire retardant is composite also can produce excellent flame retardant effect.
The invention discloses the secondary butyl ester flame retardant composition of a kind of triazine triphenyl phospho acid and application method thereof, the secondary butyl ester of triazine triphenyl phospho acid 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 the secondary butyl ester flame retardant composition of a kind of triazine triphenyl phospho acid.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 the secondary butyl ester flame retardant composition of a kind of triazine triphenyl phospho acid 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:
The secondary butyl ester flame retardant composition of a kind of triazine triphenyl phospho acid, 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 the secondary butyl ester (being called for short TTPS) of triazine triphenyl phospho acid of 10-dihydro-9-oxy obtain, and the weight fraction of TTPS 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 TTPS 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 TTPS 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 is not containing 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 TTPS, 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 TTPS and MCA and DOPO is composite to the fire-retardant data of PET
Embodiment 2 adds TTPS, 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 TTPS and MCA and PEMS is composite to the fire-retardant data of PET
Embodiment 3 adds TTPS, 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 TTPS and MPP and DOPO is composite to the fire-retardant data of PET
Embodiment 4 adds TTPS, 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 TTPS and MPP and PEMS is composite to the fire-retardant data of PET
Embodiment 5 adds TTPS, MCA, DOPO 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 6 with HC900-2 type oxygen index measurer.
Table 6 TTPS and MCA, DOPO and PEMS are composite to the fire-retardant data of PET
Embodiment 6 adds TTPS, MPP, DOPO 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 7 with HC900-2 type oxygen index measurer.
Table 7 TTPS and MPP, DOPO and PEMS are composite to the fire-retardant data of PET
Embodiment 7 adds TTPS, 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 TTPS and MCA, MPP, DOPO and PEMS are composite to the fire-retardant data of PET
Embodiment 8 adds TTPS, 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 TTPS and MCA and DOPO is composite to the fire-retardant data of PBT
Embodiment 9 adds TTPS, 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 TTPS and MCA and PEMS is composite to the fire-retardant data of PBT
Embodiment 10 adds TTPS, 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 TTPS and MPP and DOPO is composite to the fire-retardant data of PBT
Embodiment 11 adds TTPS, 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 TTPS and MPP and PEMS is composite to the fire-retardant data of PBT
Embodiment 12 adds TTPS, 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 TTPS and MCA, DOPO and PEMS are composite to the fire-retardant data of PBT
Embodiment 13 adds TTPS, 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 TTPS and MPP, DOPO and PEMS are composite to the fire-retardant data of PBT
Embodiment 14 adds TTPS, 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 TTPS and MCA, MPP, DOPO and PEMS are composite to the fire-retardant data of PBT
Claims (2)
1. the secondary butyl ester flame retardant composition of triazine triphenyl phospho acid, 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 mixes 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 with the secondary butyl ester (being called for short TTPS) of triazine triphenyl phospho acid is composite with arbitrary proportion, Homogeneous phase mixing obtained, and the weight fraction of TTPS is greater than zero
Wherein the structure of TTPS 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. the application method of the secondary butyl ester flame retardant composition of a kind of triazine triphenyl phospho acid is according to claim 1: in polyester PET or PBT, add TTPS, MCA and DOPO of different ratios or TTPS, MCA and PEMS or TTPS, MPP and DOPO or TTPS, MPP and PEMS or TTPS, MCA, DOPO and PEMS or TTPS, MPP, DOPO and PEMS or TTPS, MCA, MPP, DOPO and PEMS, mix, injection moulding or extrude under melt temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748091A (en) * | 2020-06-18 | 2020-10-09 | 浙江恒澜科技有限公司 | P-N-Si synergistic flame-retardant polyamide 6 and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3410809A (en) * | 1965-05-28 | 1968-11-12 | Monsanto Res Corp | Cn compounds |
| WO2006130353A2 (en) * | 2005-05-31 | 2006-12-07 | Eastman Kodak Company | Light-emitting device containing bis-phosphineoxide compound |
| CN103265578A (en) * | 2013-06-05 | 2013-08-28 | 苏州科技学院 | Triazinyl triphenyl sec-butyl phosphinate compound and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3410809A (en) * | 1965-05-28 | 1968-11-12 | Monsanto Res Corp | Cn compounds |
| WO2006130353A2 (en) * | 2005-05-31 | 2006-12-07 | Eastman Kodak Company | Light-emitting device containing bis-phosphineoxide compound |
| CN103265578A (en) * | 2013-06-05 | 2013-08-28 | 苏州科技学院 | Triazinyl triphenyl sec-butyl phosphinate compound and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| W. HEWERTSON ET AL.: "1,3,5-Triazines. III. Arbuzov reactions of chlorotriazines", 《JOURNAL OF THE CHEMICAL SOCIETY》 * |
| 王彦林，等: "2,4,6-三(O,O-二甲基磷酰基)-1,3,5-三嗪的合成及表征", 《兰州理工大学学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111748091A (en) * | 2020-06-18 | 2020-10-09 | 浙江恒澜科技有限公司 | P-N-Si synergistic flame-retardant polyamide 6 and preparation method thereof |
| CN111748091B (en) * | 2020-06-18 | 2022-07-08 | 浙江恒逸石化研究院有限公司 | P-N-Si synergistic flame-retardant polyamide 6 and preparation method thereof |
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