CN104194040A - Tetra(0-isopropyl-phenylphosphinyl)glycoluril (TIPRPG) flame retardant composition and application method thereof - Google Patents
Tetra(0-isopropyl-phenylphosphinyl)glycoluril (TIPRPG) flame retardant composition and application method thereof Download PDFInfo
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- CN104194040A CN104194040A CN201410397522.XA CN201410397522A CN104194040A CN 104194040 A CN104194040 A CN 104194040A CN 201410397522 A CN201410397522 A CN 201410397522A CN 104194040 A CN104194040 A CN 104194040A
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Abstract
The invention relates to a tetra(0-isopropyl-phenylphosphinyl)glycoluril (TIPRPG) flame retardant composition. The flame retardant composition is prepared from tetra(0-isopropyl-phenylphosphinyl)glycoluril 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 TIPRPG 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-sec.-propyl-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
Polyester has obtained fast development as chemical fibre industry and engineering plastics industry.At present, the throughput of China's polyester occupies the first in the world, and meanwhile China is also maximum in the world polyester consumption market, but polyester is flame-retardant modified less.Present China polyester flame-retardant degree of modification approximately 1%, and developed country's polyester flame-retardant degree of modification is 10-15%, polyester flame-retardant modification has very large development space.The deficiencies such as current polyester is high by fire retardant ubiquity price, poor performance.By composite generation cooperative flame retardant effect, thereby reduce costs, improve flame retardant properties, be an important research direction.
The invention discloses a kind of four (0-sec.-propyl-phenyl time phosphono) glycoluril flame retardant composition, four in this flame retardant composition (0-sec.-propyl-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-sec.-propyl-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-sec.-propyl-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-sec.-propyl-phenyl time phosphono) glycoluril flame retardant composition; it be by four (0-sec.-propyl-phenyl time phosphono) glycoluril (TIPRPG) 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-sec.-propyl-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 TIPRPG 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-sec.-propyl-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 TIPRPG 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 TIPRPG 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 TIPRPG to PET
Embodiment 2 adds TIPRPG 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 TIPRPG and MCA
Table 3 can find out, when 12 parts of TIPRPG and 8 parts of composite uses of MCA, limiting oxygen index(LOI) has improved 3 during than the independent use of TIPRPG, reaches 30, has well fire-retardant collaborative usefulness.And MCA is more cheap, can reduce costs.
Embodiment 3 adds TIPRPG 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 TIPRPG and MPP
Table 4 can find out, when 12 parts of TIPRPG and 8 parts of composite uses of MPP, limiting oxygen index(LOI) has improved 2 during than the independent use of TIPRPG, reaches 29, has good cooperative flame retardant usefulness.
Embodiment 4 adds the TIPRPG 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 TIPRPG and the 1240 composite flame retardant propertiess to PET
Table 5 can find out, when 12 parts of TIPRPG and 8 part of 1240 composite use, limiting oxygen index(LOI) has improved 3 during than the independent use of TIPRPG, reaches 30, 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 TIPRPG and 1240 compositely can reduce by 1240 consumption, reduce costs, and can produce good cooperative flame retardant effect.
Embodiment 5 adds TIPRPG, 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 TIPRPG, MCA and MPP
Table 6 can find out, 12 parts of TIPRPG, 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 TIPRPG, reaches 30, has good cooperative flame retardant usefulness.
Embodiment 6 adds TIPRPG, 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 TIPRPG, MCA and the 1240 composite flame retardant propertiess to PET
Table 7 can find out, when 12 parts of TIPRPG, 4 parts of MCA and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TIPRPG, 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 TIPRPG, 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 TIPRPG, MPP and the 1240 composite flame retardant propertiess to PET
Table 8 can find out, when 12 parts of TIPRPG, 4 parts of MPP and 4 part 1240 and composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TIPRPG, 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 TIPRPG, MCA, the MPP and 1240 of different ratios in polyester PET, 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 9.
Table 9 fire retardant TIPRPG, MCA, MPP and the 1240 composite flame retardant propertiess to PET
Table 9 can find out, when 10 parts of TIPRPG, 4 parts of MCA, 4 parts of MPP and 2 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TIPRPG, reaches 31, 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 TIPRPG 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 TIPRPG to PBT
Embodiment 10 adds TIPRPG, 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 TIPRPG, MCA and MPP
Table 11 can find out, when 12 parts of TIPRPG, 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 TIPRPG, reaches 30, has good cooperative flame retardant usefulness.
Embodiment 11 adds TIPRPG, 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 TIPRPG, MCA and the 1240 composite flame retardant propertiess to PBT
Table 12 can find out, when 12 parts of TIPRPG, 4 parts of MCA and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TIPRPG, 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 TIPRPG, 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 TIPRPG, MPP and the 1240 composite flame retardant propertiess to PBT
Table 13 can find out, when 12 parts of TIPRPG, 4 parts of MPP and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TIPRPG, 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 TIPRPG, 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 TIPRPG, MCA, MPP and the 1240 composite flame retardant propertiess to PBT
Table 14 can find out, when 10 parts of TIPRPG, 4 parts of MCA, 4 parts of MPP and 2 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TIPRPG, reaches 31, 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-sec.-propyl-phenyl time phosphono) glycoluril flame retardant composition; it is characterized in that; this flame retardant composition be by four (0-sec.-propyl-phenyl time phosphono) glycoluril (TIPRPG) 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-sec.-propyl-phenyl) glycoluril weight fraction in flame retardant composition is greater than zero.
Wherein, the structure of TIPRPG 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-sec.-propyl-phenyl time phosphono) glycoluril flame retardant composition is according to claim 1: in polyester PET or PBT, add the TIPRPG of different ratios and MCA or TIPRPG and MPP or TIPRPG and 1240 or TIPRPG, MCA and MPP or TIPRPG, MCA and 1240 or TIPRPG, MPP and 1240 or TIPRPG, MCA, MPP and 1240; mix injection moulding or extrude processing under melt temperature.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175778A (en) * | 2015-10-30 | 2015-12-23 | 吉林大学 | Application of organic metal phosphonic acid compound ZnCPN in aspect of synergetic fire retardant |
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 |
| CN103396448A (en) * | 2013-08-01 | 2013-11-20 | 苏州科技学院相城研究院 | Fire retardant tetra(O-isopropyl-phenyl phosphinic acyl)glycoluril compound and preparation method thereof |
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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 |
| CN103396448A (en) * | 2013-08-01 | 2013-11-20 | 苏州科技学院相城研究院 | Fire retardant tetra(O-isopropyl-phenyl phosphinic acyl)glycoluril compound and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175778A (en) * | 2015-10-30 | 2015-12-23 | 吉林大学 | Application of organic metal phosphonic acid compound ZnCPN in aspect of synergetic fire retardant |
| CN105175778B (en) * | 2015-10-30 | 2017-11-28 | 吉林大学 | A kind of applications of organic metal phosphinic acid compounds ZnCPN in terms of synergistic flame retardant |
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