CN104177650A - Tetra(0-ethyl-phenylphosphinyl)glycoluril flame retardant composition and application method thereof - Google Patents
Tetra(0-ethyl-phenylphosphinyl)glycoluril flame retardant composition and application method thereof Download PDFInfo
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- CN104177650A CN104177650A CN201410397523.4A CN201410397523A CN104177650A CN 104177650 A CN104177650 A CN 104177650A CN 201410397523 A CN201410397523 A CN 201410397523A CN 104177650 A CN104177650 A CN 104177650A
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Abstract
The invention relates to a tetra(0-ethyl-phenylphosphinyl)glycoluril flame retardant composition. The flame retardant composition is prepared from tetra(0-ethyl-phenylphosphinyl)glycoluril (TEPG) and any one or two or three of melamine cyanurate (MCA), melamine polyphosphate (MPP) and diethyl aluminum phosphinate (1240) through compounding according to any weight ratio and uniformly mixing, wherein the weight fraction of tetra(0-ethyl-phenylphosphinyl)glycoluril in the flame retardant composition is greater than 0. The flame retardant composition disclosed by the invention has the advantages that multiple elements are synergic, the material compatibility is good, the flame retardance is high, the flame retardant composition is halogen-free and environment-friendly, the application cost can be reduced and the like, so that the flame retardant composition can be applied to flame retardants of polyester, polyamide and the like.
Description
Technical field
The present invention relates to a kind of four (0-ethyl-phenyl time phosphono) glycoluril flame retardant composition and application method thereof, this flame retardant composition can be used for the fire-retardant of the engineering plastics such as polyester, polymeric amide.
Background technology
Trevira is a kind of synthon with fastest developing speed in various synthon, output is the highest, application surface is the widest, is described as the king of the fiber that is 21 century.It,, with the excellent performance such as its high strength, dimensional stabilizing, resistance to chemical attack, has purposes very widely aspect clothes, carpet and furnishing fabric, in recent years along with scientific and technical development, polyester material is also applied more and more as engineering plastics.But polyester belongs to combustible matl, polyester material is carried out to fire-retardantization processing, improve the security of polyester material, become very important research topic.Most polyester fire-retardant is by the composite realization of fire retardant, and phosphorus-nitrogen containing flame retardant has the advantages such as Halogen, low toxicity, physical and mechanical property be good, is the emphasis of paying close attention to the most in flame retardant polyester research.
The invention discloses a kind of four (0-ethyl-phenyl time phosphono) glycoluril flame retardant composition, four in this flame retardant composition (0-ethyl-phenyl time phosphono) glycoluril has symmetrical C
6h
5-P-N-C-N-P-C
6h
5large conjugation is mixed imide structure, contains many many nitrogen of phosphorus ignition-proof elements.Its composition cooperative flame retardant is effective, and stability is high, has good consistency with macromolecular material, is adapted to high temperature process, does not reduce the physical strength of material.This flame retardant composition preparation method is simple simultaneously, can reduce costs, and has good application prospect.
Summary of the invention
One of object of the present invention is to propose a kind of four (0-ethyl-phenyl time phosphono) glycoluril flame retardant composition.This flame retardant composition cooperative flame retardant usefulness is high, halogen-free environmental, and the fire retardant for polyester, polymeric amide etc., can overcome prior art deficiency, has good application and development prospect.
Another object of the present invention is to propose a kind of four (0-ethyl-phenyl time phosphono) glycoluril flame retardant composition application method in polyester PET and PBT.
For achieving the above object, the present invention has adopted following technical scheme:
A kind of four (0-ethyl-phenyl time phosphono) glycoluril flame retardant composition; it be by four (0-ethyl-phenyl time phosphono) glycoluril (TEPG) with melamine cyanurate (MCA), melamine polyphosphate (MPP) and diethyl phospho acid aluminium (1240) in any one, two or three by making composite, even mixing of weight ratio arbitrarily, and four (the inferior phosphono of 0-ethyl-phenyl) glycoluril weight fraction in flame retardant composition is greater than zero.But consider reduction and the flame retardant properties of price, the compound proportion that recommendation tables 1 is explained.Table 1 accounts for the per-cent of flame retardant composition weight for each component.
Each formulation ratio table of table 1 composite flame-retardant agent
Wherein the structure of four (0-ethyl-phenyl time phosphono) glycoluril is shown below:
The structure of MCA is shown below:
The structure of MPP is shown below:
1240 structure is shown below:
The application method of flame retardant composition of the present invention, is characterized in that as mentioned above, and the method is:
In polyester PET or PBT, add formula 1, formula 2, formula 3, formula 4, formula 5, formula 6 or formula 7 flame retardant composition, mix, injection moulding or the processing such as extrude under melt temperature.
Compared with prior art, beneficial effect of the present invention is:
(1) four in flame retardant composition component of the present invention (0-ethyl-phenyl time phosphono) glycoluril is compounds nitrogenous, the two ignition-proof elements of phosphorus, and its many phosphorus, many nitrogen make this fire retardant have good flame retardant properties; Molecule has symmetrical C
6h
5-P-N-C-N-P-C
6h
5large conjugation is mixed imide structure, polyester structure, and itself and other composition components is easy to compatibility, and has good consistency with macromolecular material, is easy to disperse, and does not separate out, and does not reduce the physical strength of material.
(2) flame retardant composition of the present invention is not halogen-containing, meets environmental requirement, has good application and development prospect.
(3) flame retardant composition of the present invention, contains phosphorus, nitrogen or aluminium element, can produce synergistic fire retardation, and polyester PET and PBT etc. is had to good flame-retarded efficiency.
(4) preparation method of flame retardant composition of the present invention is simple, and facility investment is few, can greatly reduce expensive 1240 consumption during with 1240 composite use, and can reduce production costs, and application is convenient.
(5) when flame retardant composition of the present invention has the charcoal of having of one's own effect burning, do not drip, become carbon flame-proof performance good.
Embodiment
Provide embodiment below so that the invention will be further described, in order to contrast the effect of composite flame-retardant agent, also provided the embodiment that one-component TEPG applies in polyester.But be pointed out that following examples can not be interpreted as limiting the scope of the invention, some nonessential improvement that the person skilled in the art of this area foregoing according to the present invention is made the present invention and adjustment still belong to protection scope of the present invention.
Embodiment 1 adds the TEPG of different ratios in polyester PET, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 2.
The flame retardant properties of table 2 fire retardant TEPG to PET
Embodiment 2 adds TEPG and the MCA of different ratios in polyester PET, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 3.
The composite flame retardant properties to PET of table 3 fire retardant TEPG and MCA
Table 3 can find out, when 12 parts of TEPG and 8 parts of composite uses of MCA, limiting oxygen index(LOI) has improved 3 during than the independent use of TEPG, reaches 30, has well fire-retardant collaborative usefulness.And MCA is more cheap, can reduce costs.
Embodiment 3 adds TEPG and the MPP of different ratios in polyester PET, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 4.
The composite flame retardant properties to PET of table 4 fire retardant TEPG and MPP
Table 4 can find out, when 12 parts of TEPG and 8 parts of composite uses of MPP, limiting oxygen index(LOI) has improved 3 during than the independent use of TEPG, reaches 30, has good cooperative flame retardant usefulness.
Embodiment 4 adds the TEPG and 1240 of different ratios in polyester PET, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 5.
Table 5 fire retardant TEPG and the 1240 composite flame retardant propertiess to PET
Table 5 can find out, when 12 parts of TEPG and 8 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TEPG, reaches 31, and performance has good cooperative flame retardant synergism.When the consumption when 1240 increases, flame retardant effect is more obvious.But 1240 price is very expensive, thereby TEPG and 1240 compositely can reduce by 1240 consumption, reduce costs, and can produce good cooperative flame retardant effect.
Embodiment 5 adds TEPG, MCA and the MPP of different ratios in polyester PET, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 6.
The composite flame retardant properties to PET of table 6 fire retardant TEPG, MCA and MPP
Table 6 can find out, 12 parts of TEPG, 4 parts of MCA and 4 parts of MPP are composite, and during use, limiting oxygen index(LOI) has improved 3 during than the independent use of TEPG, reaches 30, has good cooperative flame retardant usefulness.
Embodiment 6 adds TEPG, the MCA and 1240 of different ratios in polyester PET, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 7.
Table 7 fire retardant TEPG, MCA and the 1240 composite flame retardant propertiess to PET
Table 7 can find out, when 12 parts of TEPG, 4 parts of MCA and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TEPG, reaches 31, has good cooperative flame retardant usefulness.When the consumption of MCA and 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, during application, should reduce by 1240 consumption as far as possible.
Embodiment 7 adds TEPG, the MPP and 1240 of different ratios in polyester PET, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 8.
Table 8 fire retardant TEPG, MPP and the 1240 composite flame retardant propertiess to PET
Table 8 can find out, when 12 parts of TEPG, 4 parts of MPP and 4 part 1240 and composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TEPG, reaches 31, has good cooperative flame retardant usefulness.When the consumption of MPP and 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, during application, should reduce by 1240 consumption as far as possible.
Embodiment 8 adds TEPG, MCA, the MPP and 1240 of different ratios in polyester PET, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 9.
Table 9 fire retardant TEPG, MCA, MPP and the 1240 composite flame retardant propertiess to PET
Table 9 can find out, when 10 parts of TEPG, 4 parts of MCA, 4 parts of MPP and 2 part of 1240 composite use, limiting oxygen index(LOI) has improved 5 during than the independent use of TEPG, reaches 32, has good cooperative flame retardant usefulness.When the consumption when 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, during application, should reduce by 1240 consumption as far as possible.
Embodiment 9 adds the TEPG of different ratios in polyester PBT, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 10.
The flame retardant properties of table 10 fire retardant TEPG to PBT
Embodiment 10 adds TEPG, MCA and the MPP of different ratios in polyester PBT, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 11.
The composite flame retardant properties to PBT of table 11 fire retardant TEPG, MCA and MPP
Table 11 can find out, when 12 parts of TEPG, 4 parts of MCA and 4 parts of composite uses of MPP, limiting oxygen index(LOI) has improved 3 during than the independent use of TEPG, reaches 30, has good cooperative flame retardant usefulness.
Embodiment 11 adds TEPG, the MCA and 1240 of different ratios in polyester PBT, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 12.
Table 12 fire retardant TEPG, MCA and the 1240 composite flame retardant propertiess to PBT
Table 12 can find out, when 12 parts of TEPG, 4 parts of MCA and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TEPG, reaches 31, has good cooperative flame retardant usefulness.When the consumption of MCA and 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, during application, should reduce by 1240 consumption as far as possible.
Embodiment 12 adds TEPG, the MPP and 1240 of different ratios in polyester PBT, mixes, and with XJ-01 type forcing machine, extrudes the batten of diameter 3mm under melt temperature, with HC900-2 type oxygen index measurer, surveys its limiting oxygen index(LOI), the results are shown in Table 13.
Table 13 fire retardant TEPG, MPP and the 1240 composite flame retardant propertiess to PBT
Table 13 can find out, when 12 parts of TEPG, 4 parts of MPP and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TEPG, reaches 31, has good cooperative flame retardant usefulness.When the consumption of MPP and 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, during application, should reduce by 1240 consumption as far as possible.
Embodiment 13 adds TEPG, MCA, the MPP and 1240 of different ratios in polyester PBT, mix, with XJ-01 type forcing machine, under melt temperature, extrude the batten of diameter 3mm, with HC900-2 type oxygen index measurer, survey its limiting oxygen index(LOI), the results are shown in Table 14.
Table 14 fire retardant TEPG, MCA, MPP and the 1240 composite flame retardant propertiess to PBT
Table 14 can find out, when 10 parts of TEPG, 4 parts of MCA, 4 parts of MPP and 2 part of 1240 composite use, limiting oxygen index(LOI) has improved 5 during than the independent use of TEPG, reaches 32, has good cooperative flame retardant usefulness.When the consumption when 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, during application, should reduce by 1240 consumption as far as possible.
Claims (2)
1. one kind four (0-ethyl-phenyl time phosphono) glycoluril flame retardant composition; it is characterized in that; this flame retardant composition be by four (0-ethyl-phenyl time phosphono) glycoluril (TEPG) with melamine cyanurate (MCA), melamine polyphosphate (MPP) and diethyl phospho acid aluminium (1240) in any one, two or three by making composite, even mixing of weight ratio arbitrarily, and four (the inferior phosphono of 0-ethyl-phenyl) glycoluril weight fraction in flame retardant composition is greater than zero.
Wherein, the structure of TEPG is shown below:
The structure of MCA is shown below:
The structure of MPP is shown below:
1240 structure is shown below:
2. the application method of a kind of four (0-ethyl-phenyl time phosphono) glycoluril flame retardant composition is according to claim 1: in polyester PET or PBT, add the TEPG of different ratios and MCA or TEPG and MPP or TEPG and 1240 or TEPG, MCA and MPP or TEPG, MCA and 1240 or TEPG, MPP and 1240 or TEPG, MCA, MPP and 1240; mix injection moulding or extrude processing under melt temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410397523.4A CN104177650B (en) | 2014-08-14 | Four (O-Ethyl-phenyl time phosphono) glycoluril fire retardant combination and application processes thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410397523.4A CN104177650B (en) | 2014-08-14 | Four (O-Ethyl-phenyl time phosphono) glycoluril fire retardant combination and application processes thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104177650A true CN104177650A (en) | 2014-12-03 |
| CN104177650B CN104177650B (en) | 2016-11-30 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103109002A (en) * | 2010-09-23 | 2013-05-15 | 英威达技术有限公司 | Flame retardant fibers, yarns, and fabrics made therefrom |
| CN103396449A (en) * | 2013-08-01 | 2013-11-20 | 苏州科技学院相城研究院 | Fire retardant tetra(0-ethyl-phenyl phosphinic acyl)glycoluril compound and preparation method thereof |
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103109002A (en) * | 2010-09-23 | 2013-05-15 | 英威达技术有限公司 | Flame retardant fibers, yarns, and fabrics made therefrom |
| CN103396449A (en) * | 2013-08-01 | 2013-11-20 | 苏州科技学院相城研究院 | Fire retardant tetra(0-ethyl-phenyl phosphinic acyl)glycoluril compound and preparation method thereof |
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