CN104130557A - Tetra(0,0-dipropylphosphoryl)glycoluril (TPRG) flame retardant composition and application method thereof - Google Patents
Tetra(0,0-dipropylphosphoryl)glycoluril (TPRG) flame retardant composition and application method thereof Download PDFInfo
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- CN104130557A CN104130557A CN201410397729.7A CN201410397729A CN104130557A CN 104130557 A CN104130557 A CN 104130557A CN 201410397729 A CN201410397729 A CN 201410397729A CN 104130557 A CN104130557 A CN 104130557A
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Abstract
The invention relates to a tetra(0,0-dipropylphosphoryl)glycoluril (TPRG) flame retardant composition. The flame retardant composition is prepared by compounding and uniformly mixing TPRG with any one, two or three of melamine cyanurate (MCA), melamine pyrophosphate (MPP) and diethyl aluminium phosphinate (1240) according to a random weight ratio, wherein the weight fraction of TPRG in the flame retardant composition is more than zero. The flame retardant composition has the advantages of multielement synergy, good compatibility with materials, high flame retardance, no halogen, environment friendliness, capability of reducing the application cost and the like, and can be used as the flame retardant of polyesters, polyamides and the like.
Description
Technical field
The present invention relates to a kind of four (0,0-dipropyl phosphoryl) 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 industrial is an industry closely bound up with national economy.Its product is widely used in all respects of the national economy such as man-made fiber, light industry, electronics, building.It is carried out to flame-retardant modified it is functional and to expand its range of application be research highly significant to improve.From the object of halogen-free flameproof, phosphorus, nitrogenated flame retardant have the advantages such as low toxicity, low cigarette, flame retardant properties be good, thereby it has become the focus development direction of polyester halogen-free flame retardants.And by multiple fire retardant composite or design molecule in multielement cooperative flame retardant improve the hot subject that its flame-retarded efficiency is also current fire retardant technical study.
The invention discloses a kind of four (0; 0-dipropyl phosphoryl) glycoluril flame retardant composition; in this flame retardant composition four (0,0-dipropyl phosphoryl) glycoluril has symmetrical P-N-C-N-P conjugation and mixes 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 (0,0-dipropyl phosphoryl) glycoluril flame retardant composition.This flame retardant composition cooperative flame retardant usefulness is high, and halogen-free environmental, for polyester flame-retardant agent, polymeric amide fire retardant etc., can meet environmental requirement, has good application and development prospect.
Another object of the present invention is to propose a kind of four (0,0-dipropyl phosphoryl) 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; 0-dipropyl phosphoryl) glycoluril flame retardant composition; it is by four (0; 0-dipropyl phosphoryl) glycoluril (TPRG) with in melamine cyanurate (MCA), melamine polyphosphate (MPP) and diethyl phospho acid aluminium (1240) any one, two or three by composite, even mixing of weight ratio makes arbitrarily; and four (0,0-dipropyl phosphoryl) 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 is the per-cent that each component accounts for flame retardant composition weight.
The each formulation ratio table of table 1 composite flame-retardant agent
Wherein the structure of TPRG 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 (0,0-dipropyl phosphoryl) 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 P-N-C-N-P conjugation and mixes 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. are 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, 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 TPRG 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 TPRG of different ratios in polyester PET, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 2.
The flame retardant properties of table 2 fire retardant TPRG to PET
Embodiment 2 adds TPRG and the MCA of different ratios in polyester PET, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 3.
The composite flame retardant properties to PET of table 3 fire retardant TPRG and MCA
Table 3 can find out, when 12 parts of TPRG and 8 parts of composite uses of MCA, limiting oxygen index(LOI) has improved 2 during than the independent use of TPRG, reaches 30, has well fire-retardant collaborative usefulness.And MCA is more cheap, can reduce costs.
Embodiment 3 adds TPRG and the MPP of different ratios in polyester PET, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 4.
The composite flame retardant properties to PET of table 4 fire retardant TPRG and MPP
Table 4 can find out, when 12 parts of TPRG and 8 parts of composite uses of MPP, limiting oxygen index(LOI) has improved 2 during than the independent use of TPRG, reaches 30, has good cooperative flame retardant usefulness.
Embodiment 4 adds the TPRG and 1240 of different ratios in polyester PET, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 5.
Table 5 fire retardant TPRG and the 1240 composite flame retardant propertiess to PET
Table 5 can find out, when 12 parts of TPRG and 8 part of 1240 composite use, limiting oxygen index(LOI) has improved 3 during than the independent use of TPRG, reaches 31, and performance has good cooperative flame retardant synergism.When consumption when 1240 increases, flame retardant effect is more obvious.But 1240 price is very expensive, thereby TPRG and 1240 compositely can reduce by 1240 consumption, reduce costs, and can produce good cooperative flame retardant effect.
Embodiment 5 adds TPRG, MCA and the MPP of different ratios in polyester PET, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 6.
The composite flame retardant properties to PET of table 6 fire retardant TPRG, MCA and MPP
Table 6 can find out, 12 parts of TPRG, 4 parts of MCA and 4 parts of MPP are composite, and when use, limiting oxygen index(LOI) has improved 3 during than the independent use of TPRG, reaches 31, has good cooperative flame retardant usefulness.
Embodiment 6 adds TPRG, the MCA and 1240 of different ratios in polyester PET, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 7.
Table 7 fire retardant TPRG, MCA and the 1240 composite flame retardant propertiess to PET
Table 7 can find out, when 12 parts of TPRG, 4 parts of MCA and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 3 during than the independent use of TPRG, reaches 31, has good cooperative flame retardant usefulness.In the time that the consumption of MCA and 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, when application, should reduce by 1240 consumption as far as possible.
Embodiment 7 adds TPRG, the MPP and 1240 of different ratios in polyester PET, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 8.
Table 8 fire retardant TPRG, MPP and the 1240 composite flame retardant propertiess to PET
Table 8 can find out, when 12 parts of TPRG, 4 parts of MPP and 4 part 1240 and composite use, limiting oxygen index(LOI) has improved 3 during than the independent use of TPRG, reaches 31, has good cooperative flame retardant usefulness.In the time that the consumption of MPP and 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, when application, should reduce by 1240 consumption as far as possible.
Embodiment 8 adds TPRG, MCA, the MPP and 1240 of different ratios in polyester PET, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 9.
Table 9 fire retardant TPRG, MCA, MPP and the 1240 composite flame retardant propertiess to PET
Table 9 can find out, when 10 parts of TPRG, 4 parts of MCA, 4 parts of MPP and 2 part of 1240 composite use, limiting oxygen index(LOI) has improved 3 during than the independent use of TPRG, reaches 31, has good cooperative flame retardant usefulness.When consumption when 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, when application, should reduce by 1240 consumption as far as possible.
Embodiment 9 adds the TPRG of different ratios in polyester PBT, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 10.
The flame retardant properties of table 10 fire retardant TPRG to PBT
Embodiment 10 adds TPRG, MCA and the MPP of different ratios in polyester PBT, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 11.
The composite flame retardant properties to PBT of table 11 fire retardant TPRG, MCA and MPP
Table 11 can find out, when 12 parts of TPRG, 4 parts of MCA and 4 parts of composite uses of MPP, limiting oxygen index(LOI) has improved 2 during than the independent use of TPRG, reaches 30, has good cooperative flame retardant usefulness.
Embodiment 11 adds TPRG, the MCA and 1240 of different ratios in polyester PBT, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 12.
Table 12 fire retardant TPRG, MCA and the 1240 composite flame retardant propertiess to PBT
Table 12 can find out, when 12 parts of TPRG, 4 parts of MCA and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 3 during than the independent use of TPRG, reaches 31, has good cooperative flame retardant usefulness.In the time that the consumption of MCA and 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, when application, should reduce by 1240 consumption as far as possible.
Embodiment 12 adds TPRG, the MPP and 1240 of different ratios in polyester PBT, mixes, and extrudes the batten of diameter 3mm with XJ-01 type forcing machine under melt temperature, surveys its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 12.
Table 13 fire retardant TPRG, MPP and the 1240 composite flame retardant propertiess to PBT
Table 13 can find out, when 12 parts of TPRG, 4 parts of MPP and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 3 during than the independent use of TPRG, reaches 31, has good cooperative flame retardant usefulness.In the time that the consumption of MPP and 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, when application, should reduce by 1240 consumption as far as possible.
Embodiment 13 adds TPRG, MCA, the MPP and 1240 of different ratios in polyester PBT, mix, under melt temperature, extrude the batten of diameter 3mm with XJ-01 type forcing machine, survey its limiting oxygen index(LOI) with HC900-2 type oxygen index measurer, the results are shown in Table 14.
Table 14 fire retardant TPRG, MCA, MPP and the 1240 composite flame retardant propertiess to PBT
Table 14 can find out, when 10 parts of TPRG, 4 parts of MCA, 4 parts of MPP and 2 part of 1240 composite use, limiting oxygen index(LOI) has improved 3 during than the independent use of TPRG, reaches 31, has good cooperative flame retardant usefulness.When consumption when 1240 increases, flame retardant effect can be better, but due to 1240 costlinesses, consider cost, when application, should reduce by 1240 consumption as far as possible.
Claims (2)
1. one kind four (0; 0-dipropyl phosphoryl) glycoluril flame retardant composition; it is characterized in that; this flame retardant composition is by four (0; 0-dipropyl phosphoryl) glycoluril (TPRG) with in melamine cyanurate (MCA), melamine polyphosphate (MPP) and diethyl phospho acid aluminium (1240) any one, two or three by composite, even mixing of weight ratio makes arbitrarily; and four (0,0-dipropyl phosphoryl) glycoluril weight fraction in flame retardant composition is greater than zero.
Wherein, the structure of TPRG is shown below:
The structure of MCA is shown below:
The structure of MPP is shown below:
1240 structure is shown below:
2. according to claim 1 a kind of four (0; 0-dipropyl phosphoryl) application method of glycoluril flame retardant composition is: in polyester PET or PBT, add the TPRG of different ratios and MCA or TPRG and MPP or TPRG and 1240 or TPRG, MCA and MPP or TPRG, MCA and 1240 or TPRG, MPP and 1240 or TPRG, MCA, MPP and 1240; mix injection moulding or extrude processing under melt temperature.
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