CN104231574A - Triazine triphenyl phosphinic acid butyl ester flame retardant composition and application method thereof - Google Patents
Triazine triphenyl phosphinic acid butyl ester flame retardant composition and application method thereof Download PDFInfo
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- CN104231574A CN104231574A CN201410507988.0A CN201410507988A CN104231574A CN 104231574 A CN104231574 A CN 104231574A CN 201410507988 A CN201410507988 A CN 201410507988A CN 104231574 A CN104231574 A CN 104231574A
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Abstract
The invention relates to a triazine triphenyl phosphinic acid 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 butyl ester (TTPB) at any proportion, wherein the weight part of the TTPB 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 phospho acid butyl ester 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
Along with the enhancing of people's awareness of the importance of fire prevention and the appearance of relevant flame retardant regulation, the development of halogenated flame retardant is faced with severe tests, and makes market have very strong urgency to environment friendly flame retardant, and low toxicity, efficiently fire retardant are more favored by people.Research shows that multielement synergetic organic phosphine fire retardant advantage is a lot, can give material well 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 means becoming the research of current flame-retarded technology.The nitrogenous compound being wherein carrier with stable triazine ring derivatives is introduced in flame retardant molecule, can bring highly effective flame-retardant and become charcoal effect, having obvious cooperative flame retardant effect to the flame retardant properties improving fire retardant.The phosphorus nitrogen cooperative flame retardant molecule of triazine ring structure and organic phosphine grafting Cheng Xin more can play the premium properties of halogen-free flame retardants, by also producing excellent flame retardant effect with other fire retardant is composite.
The invention discloses a kind of triazine triphenyl phospho acid butyl ester flame retardant composition and application method thereof, triazine triphenyl phospho acid butyl ester 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, and 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 triazine triphenyl phospho acid butyl ester 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 triazine triphenyl phospho acid butyl ester 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 triazine triphenyl phospho acid butyl ester 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 triazine triphenyl phospho acid butyl ester (being called for short TTPB) of 10-dihydro-9-oxy obtain, and the weight fraction of TTPB 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 TTPB 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 TTPB 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 has not given up 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 TTPB, 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 TTPB and MCA and DOPO is composite to the fire-retardant data of PET
Embodiment 2 adds TTPB, 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 TTPB and MCA and PEMS is composite to the fire-retardant data of PET
Embodiment 3 adds TTPB, 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 TTPB and MPP and DOPO is composite to the fire-retardant data of PET
Embodiment 4 adds TTPB, 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 TTPB and MPP and PEMS is composite to the fire-retardant data of PET
Embodiment 5 adds TTPB, 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 TTPB and MCA, DOPO and PEMS are composite to the fire-retardant data of PET
Embodiment 6 adds TTPB, 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 TTPB and MPP, DOPO and PEMS are composite to the fire-retardant data of PET
Embodiment 7 adds TTPB, 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 TTPB and MCA, MPP, DOPO and PEMS are composite to the fire-retardant data of PET
Embodiment 8 adds TTPB, 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 TTPB and MCA and DOPO is composite to the fire-retardant data of PBT
Embodiment 9 adds TTPB, 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 TTPB and MCA and PEMS is composite to the fire-retardant data of PBT
Embodiment 10 adds TTPB, 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 TTPB and MPP and DOPO is composite to the fire-retardant data of PBT
Embodiment 11 adds TTPB, 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 TTPB and MPP and PEMS is composite to the fire-retardant data of PBT
Embodiment 12 adds TTPB, 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 TTPB and MCA, DOPO and PEMS are composite to the fire-retardant data of PBT
Embodiment 13 adds TTPB, 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 TTPB and MPP, DOPO and PEMS are composite to the fire-retardant data of PBT
Embodiment 14 adds TTPB, 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 TTPB and MCA, MPP, DOPO and PEMS are composite to the fire-retardant data of PBT
Claims (2)
1. a triazine triphenyl phospho acid butyl ester 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 triazine triphenyl phospho acid butyl ester (being called for short TTPB), Homogeneous phase mixing obtained, and the weight fraction of TTPB is greater than zero
Wherein the structure of TTPB 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 triazine triphenyl phospho acid butyl ester flame retardant composition is according to claim 1: in polyester PET or PBT, add TTPB, MCA and DOPO of different ratios or TTPB, MCA and PEMS or TTPB, MPP and DOPO or TTPB, MPP and PEMS or TTPB, MCA, DOPO and PEMS or TTPB, MPP, DOPO and PEMS or TTPB, MCA, MPP, DOPO and PEMS, mix, injection moulding or extrude under melt temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI628186B (en) * | 2017-08-04 | 2018-07-01 | 晉一化工股份有限公司 | Phosphorus-containing flame retardant and its composition, epoxy resin composition, thermoplastic resin composition, use |
| CN111349318A (en) * | 2018-12-20 | 2020-06-30 | 财团法人纺织产业综合研究所 | Flame-retardant fiber master batch, fluorescent flame-retardant fiber composition and fluorescent flame-retardant fiber |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2685581A (en) * | 1952-10-08 | 1954-08-03 | Eastman Kodak Co | Organic phosphorus compounds |
| WO2006130353A2 (en) * | 2005-05-31 | 2006-12-07 | Eastman Kodak Company | Light-emitting device containing bis-phosphineoxide compound |
| CN101376665A (en) * | 2008-09-29 | 2009-03-04 | 四川东材科技集团股份有限公司 | Phosphaphenanthrene flame-retardant compound containing s-triazine structure, and preparation and use thereof |
| 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 CN201410507988.0A patent/CN104231574B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2685581A (en) * | 1952-10-08 | 1954-08-03 | Eastman Kodak Co | Organic phosphorus compounds |
| WO2006130353A2 (en) * | 2005-05-31 | 2006-12-07 | Eastman Kodak Company | Light-emitting device containing bis-phosphineoxide compound |
| CN101376665A (en) * | 2008-09-29 | 2009-03-04 | 四川东材科技集团股份有限公司 | Phosphaphenanthrene flame-retardant compound containing s-triazine structure, and preparation and use thereof |
| 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 (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI628186B (en) * | 2017-08-04 | 2018-07-01 | 晉一化工股份有限公司 | Phosphorus-containing flame retardant and its composition, epoxy resin composition, thermoplastic resin composition, use |
| CN111349318A (en) * | 2018-12-20 | 2020-06-30 | 财团法人纺织产业综合研究所 | Flame-retardant fiber master batch, fluorescent flame-retardant fiber composition and fluorescent flame-retardant fiber |
| CN111349318B (en) * | 2018-12-20 | 2023-01-10 | 财团法人纺织产业综合研究所 | Flame-retardant fiber master batch, fluorescent flame-retardant fiber composition and fluorescent flame-retardant fiber |
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