CN104130555A - Tetra(0,0-diphenylphosphoryl)glycoluril (TBBG) flame retardant composition and application method thereof - Google Patents
Tetra(0,0-diphenylphosphoryl)glycoluril (TBBG) flame retardant composition and application method thereof Download PDFInfo
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Abstract
The invention relates to a tetra(0,0-diphenylphosphoryl)glycoluril (TBBG) flame retardant composition. The flame retardant composition is prepared by compounding and uniformly mixing TBBG 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 TBBG 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-diphenylphosphine acyl group) 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
Along with macromolecular material is at electronic apparatus, communications and transportation, furniture, the widespread use in the fields such as upholstery, the disaster hidden-trouble that its inflammableness is brought is also more and more, has therefore promoted the development of flame retarded polymeric material technology.At present, due to the environmentally safe requirement of people, the non-halogen cry of fire retardant is more and more higher, because phosphorus-nitrogen containing flame retardant has efficiently, low toxicity, the advantages such as non-corrosiveness, have become the flame retardant series of current most study, in application, by phosphorus, the composite generation cooperative flame retardant of nitrogenated flame retardant effect, improve that it is fire-retardant, processing characteristics is one of important directions of research and development.
The invention discloses a kind of four (0; 0-diphenylphosphine acyl group) glycoluril flame retardant composition; in this flame retardant composition four (0,0-diphenylphosphine acyl group) 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-diphenylphosphine acyl group) 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-diphenylphosphine acyl group) 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-diphenylphosphine acyl group) glycoluril flame retardant composition; it is by four (0; 0-diphenylphosphine acyl group) glycoluril (TBBG) 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-diphenylphosphine acyl group) 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 TBBG 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-diphenylphosphine acyl group) 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. 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 TBBG 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 TBBG 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 TBBG to PET
Embodiment 2 adds TBBG 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 TBBG and MCA
Table 3 can find out, when 12 parts of TBBG and 8 parts of composite uses of MCA, limiting oxygen index(LOI) has improved 3 during than the independent use of TBBG, reaches 29, has well fire-retardant collaborative usefulness.And MCA is more cheap, can reduce costs.
Embodiment 3 adds TBBG 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 TBBG and MPP
Table 4 can find out, when 12 parts of TBBG and 8 parts of composite uses of MPP, limiting oxygen index(LOI) has improved 3 during than the independent use of TBBG, reaches 29, has good cooperative flame retardant usefulness.
Embodiment 4 adds the TBBG 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 TBBG and the 1240 composite flame retardant propertiess to PET
Table 5 can find out, when 12 parts of TBBG and 8 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TBBG, 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 TBBG and 1240 compositely can reduce by 1240 consumption, reduce costs, and can produce good cooperative flame retardant effect.
Embodiment 5 adds TBBG, 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 TBBG, MCA and MPP
Table 6 can find out, 12 parts of TBBG, 4 parts of MCA and 4 parts of MPP are composite, and during use, limiting oxygen index(LOI) has improved 4 during than the independent use of TBBG, reaches 30, has good cooperative flame retardant usefulness.
Embodiment 6 adds TBBG, 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 TBBG, MCA and the 1240 composite flame retardant propertiess to PET
Table 7 can find out, when 12 parts of TBBG, 4 parts of MCA and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TBBG, reaches 30, 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 TBBG, 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 TBBG, MPP and the 1240 composite flame retardant propertiess to PET
Table 8 can find out, when 12 parts of TBBG, 4 parts of MPP and 4 part 1240 and composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TBBG, reaches 30, 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 TBBG, 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 TBBG, MCA, MPP and the 1240 composite flame retardant propertiess to PET
Table 9 can find out, when 10 parts of TBBG, 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 TBBG, reaches 30, 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 TBBG 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 TBBG to PBT
Embodiment 10 adds TBBG, 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 TBBG, MCA and MPP
Table 11 can find out, when 12 parts of TBBG, 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 TBBG, reaches 29, has good cooperative flame retardant usefulness.
Embodiment 11 adds TBBG, 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 TBBG, MCA and the 1240 composite flame retardant propertiess to PBT
Table 12 can find out, when 12 parts of TBBG, 4 parts of MCA and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TBBG, reaches 30, 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 TBBG, 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 TBBG, MPP and the 1240 composite flame retardant propertiess to PBT
Table 13 can find out, when 12 parts of TBBG, 4 parts of MPP and 4 part of 1240 composite use, limiting oxygen index(LOI) has improved 4 during than the independent use of TBBG, reaches 30, 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 TBBG, 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 TBBG, MCA, MPP and the 1240 composite flame retardant propertiess to PBT
Table 14 can find out, when 10 parts of TBBG, 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 TBBG, 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; 0-diphenylphosphine acyl group) glycoluril flame retardant composition; it is characterized in that; this flame retardant composition is by four (0; 0-diphenylphosphine acyl group) glycoluril (TBBG) 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-diphenylphosphine acyl group) glycoluril weight fraction in flame retardant composition is greater than zero.
Wherein, the structure of TBBG 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-diphenylphosphine acyl group) application method of glycoluril flame retardant composition is: in polyester PET or PBT, add the TBBG of different ratios and MCA or TBBG and MPP or TBBG and 1240 or TBBG, MCA and MPP or TBBG, MCA and 1240 or TBBG, MPP and 1240 or TBBG, MCA, MPP and 1240; mix injection moulding or extrude processing under melt temperature.
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Effective date of registration: 20190529 Address after: 215011 No. 1701 Binhe Road, Suzhou High-tech Zone, Jiangsu Province (in the incubator of Science Park of Suzhou University of Science and Technology) Patentee after: Suzhou alcody new Mstar Technology Ltd Address before: 215131 Room 610, Yuanhe Building, 959 Jiayuan Road, Xiangcheng District, Suzhou City, Jiangsu Province Patentee before: Xiangcheng Institute of Suzhou University of Science and Technology |