CN104945866A - PBT (polybutylene terephthalate) molding composition - Google Patents
PBT (polybutylene terephthalate) molding composition Download PDFInfo
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- CN104945866A CN104945866A CN201510367127.1A CN201510367127A CN104945866A CN 104945866 A CN104945866 A CN 104945866A CN 201510367127 A CN201510367127 A CN 201510367127A CN 104945866 A CN104945866 A CN 104945866A
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Abstract
The invention discloses a PBT (polybutylene terephthalate) molding composition which comprises the following components in percentage by mass: 30-70% of PBT, 12-20% of halogen-free flame retardant, 1-3% of organic phosphorus nitrile compound, 0-5% of toughener and 10-40% of glass fiber. The invention aims to provide a halogen-free flame-retardant glass-fiber-reinforced PBT molding composition which has the advantages of excellent heat stability, excellent flame retardancy, no release of toxic substances, environment friendliness and high mechanical properties. After 1-3% of the organic phosphorus nitrile compound is added, the inventor surprisedly detects that the mechanical properties of the molding composition are obviously enhanced, and the mechanical properties of the molding composition start descending obviously when the consumption of the organic phosphorus nitrile is continuously increased.
Description
Technical field
The present invention relates to technical field of polymer composite materials, be specifically related to a kind of Halogen low-poison and combustion-resisting fiber glass reinforced PBT moulding compound of high-mechanical property.
Background technology
For a long time, the fire retardant that PBT (polybutylene terephthalate) flame-retardant system is continued to use mostly is halogenated flame retardant, flame-retardant PBT prepared by the method can produce a large amount of black smokes when burning, there are certain corrodibility and toxicity, in view of all drawbacks of halogenated flame retardant, European Union discloses WEEE and RoHS two instructions for 2003, the toxicity of halogen flame and the arguement of environmental problem are pushed to a new high, in the case, halogen-free environment-friendly flame-proof PBT replaces halogen system flame-retardant reinforced PBT to be the inexorable trend developed.
But along with various environmental protection instruction and the continuous of laws and regulations requirement are improved and improve, some halogen-free flame retardantss that PBT is conventional, only just accomplishing not halogen-containing, is not low toxic and environment-friendly truly.2013, the fire retardant PBT with no halogen product of certain export enterprise European Union domestic, after arriving Europe, was given heavy punishment because finding at freight container containing phosphuret-(t)ed hydrogen by sea-freight.Phosphine gas, has another name called phosphine, is a kind of colourless hypertoxic inflammable gas, can constitutes a threat to, also have corrosive nature in addition to hardware after suction to HUMAN HEALTH.
At present, some halogen-free flame retardantss that PBT is conventional on the market, some itself is that European Union environmental protection regulation limitations uses, as boron trioxide etc., some is due to the instability of chemical structure in essence, can toxic substance be produced under melt-processed and some chemical environment, as red phosphorus or inorganic phospho acid aluminium, can produce under melt-processed and some environment for use and discharge phosphine gas.And other halogen-free flame retardants, as German Clariant Exolit OP1240, its nucleus is aluminum diethylphosphinate, Heat stability is good, relevant authoritative institution of European Union lasts several years follow-up study and analyzes Exolit OP series product to the impact of human health, environment and ecology, already draw the conclusion of affirmative, but due to itself and PBT resin poor compatibility, cause the mechanical property of system to be starkly lower than the performance of traditional halogen system flame-proof glass fibre enhancing PBT.
Therefore, the thermally-stabilised difference of halogen-free flameproof product is there is in prior art, easily toxic substance is discharged in high temperature process or storage process, though or Heat stability is good, but the problem that mechanical property is on the low side, so PBT fireproof reinforced composite material how is made to possess excellent mechanical property under Halogen, low toxicity, eco-friendly prerequisite and become urgent problem meeting.
Summary of the invention
In view of this, the object of the invention is to propose a kind of PBT moulding compound, to overcome the technical problem that prior art exists.
Based on above-mentioned purpose, the invention provides, its composition comprises by massfraction:
In some embodiments of the invention, described organophosphorus nitrile compound is selected from least one in six ethoxy basic ring three phosphonitriles and hexaphenoxycyclotriphosphazene.
In some embodiments of the invention, described halogen-free flame retardants is selected from least one in organic secondary phosphine acid salt and melamine polyphosphate.
In some embodiments of the invention, described organic secondary phosphine acid salt is selected from least one in aluminum diethylphosphinate and diphenyl phosphonic acid aluminium.
In some embodiments of the invention, the limiting viscosity of described PBT is 0.7 ~ 1.1dl/g.
In some embodiments of the invention, described toughner is selected from least one in ethylene methyl methacrylate-glycidyl acrylate, glycidyl methacrylate graft polyoxyethylene.
In some embodiments of the invention, described glass fibre is the alkali free glass fibre of filament diameter 10um ~ 13um.
In some embodiments of the invention, the surface of described glass fibre is through silane coupling agent process.
In some embodiments of the invention, described PBT mold composition also comprises: oxidation inhibitor B225 and lubricant PETS, and the quality sum of described oxidation inhibitor B225 and lubricant PETS accounts for 0 ~ 2% of described PBT mold composition.
In some embodiments of the invention, described silane coupling agent is selected from 3-aminopropyl triethoxysilane or 3-(2,3-epoxy group(ing)) propyl trimethoxy silicane.
As can be seen from above, the present invention aims to provide a kind ofly to be had excellent thermostability and flame retardant properties, not to discharge toxic substance, environmental friendliness, and the high halogen-free flame-retardant glass fiber of mechanical property strengthens PBT moulding compound.In the present invention, after the organophosphorus nitrile compound of interpolation 1% ~ 3%, the mechanical property of the discovery moulding compound that contriver is surprised obtains significant raising, and continues the consumption strengthening organic phosphonitrile, and the mechanical property of moulding compound but starts obvious decline.Visible, the special construction of organophosphorus nitrile compound significantly improves organic secondary phosphine acid salt and trimeric cyanamide polyphosphonic acid and receives the consistency of halogen-free flame retardants system and PBT resin, and the mechanical property of moulding compound is improved.But when addition continues to increase, the more embodiments of organophosphorus nitrile compound be flame retardant properties, and due to the plastification of organophosphorus nitrile compound, cause moulding compound mechanical property to decline.
The invention has the beneficial effects as follows:
(1) PBT moulding compound of the present invention is not halogen-containing, and excellent fireproof performance;
(2) from the viewpoint of environmental protection, PBT moulding compound of the present invention produces without toxic substance in high temperature process or when storing, and meets European Union environmental protection requirement completely;
(3) PBT moulding compound mechanical property of the present invention is high, close to the level that the PBT bromine antimony fire retardant material of current main flow is suitable;
(4) moulding compound preparation method of the present invention is simple, high machinery performance halogen-free low-poison and combustion-resisting fiber glass reinforced PBT moulding compound is prepared by each component being used for PBT moulding compound mutually being mixed, conventional dry blend melting granulating technology can be adopted, without any special restriction.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, the present invention is described in more detail.
Embodiment 1
As one embodiment of the present of invention, the preparation method of described PBT mold composition comprises the following steps:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 6040g, the aluminum diethylphosphinate 1850g of 1.03dl/g, hexaphenoxycyclotriphosphazene 300g, ethylene methyl methacrylate-glycidyl acrylate 300g, filament diameter are 13um the alkali free glass fibre 1500g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) by PBT resin dry 4h at 120 DEG C, by aluminum diethylphosphinate, alkoxycyclotriphosphderivative, ethylene-methyl acrylate-methyl methacrylate copolymer, oxidation inhibitor B225 and lubricant PETS mixes with PBT resin and is placed on twin screw extruder (diameter 35mm, length-to-diameter ratio 32) in, the feeding rotating speed controlling twin screw extruder controls at 350rpm, each zone temperature remains on 205 DEG C ~ 230 DEG C, screw speed 350rpm, in forcing machine downstream, glass fiber opening adds glass fibre, vacuum pump on forcing machine controls the vacuum tightness≤-0.06MPa in forcing machine, pass through melting, mixing, extrude, cooling, dry, pelletizing obtains product.
Embodiment 2
As one embodiment of the present of invention, the preparation method of described PBT mold composition comprises the following steps:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 6090g, the diphenyl phosphonic acid aluminium 1850g of 1.03dl/g, six ethoxy basic ring three phosphonitrile 200g, ethylene methyl methacrylate-glycidyl acrylate 300g, filament diameter are 13um the alkali free glass fibre 1500g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Embodiment 3
As one embodiment of the present of invention, the preparation method of described PBT mold composition comprises the following steps:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 6140g, the melamine polyphosphate 1900g of 1.03dl/g, hexaphenoxycyclotriphosphazene 100g, ethylene methyl methacrylate-glycidyl acrylate 300g, filament diameter are 13um the alkali free glass fibre 1500g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Comparative example 1:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 6040g, the aluminum diethylphosphinate 2100g of 1.03dl/g, ethylene methyl methacrylate-glycidyl acrylate 300g, filament diameter are 13um the alkali free glass fibre 1500g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Comparative example 2:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 6240g, the aluminum diethylphosphinate 2090g of 1.03dl/g, hexaphenoxycyclotriphosphazene 10g, ethylene methyl methacrylate-glycidyl acrylate 300g, filament diameter are 13um the alkali free glass fibre 1500g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Comparative example 3:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 5940g, the aluminum diethylphosphinate 1600g of 1.03dl/g, hexaphenoxycyclotriphosphazene 500g, ethylene methyl methacrylate-glycidyl acrylate 300g, filament diameter are 13um the alkali free glass fibre 1500g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
The Halogen low-poison and combustion-resisting PBT reinforced composite that embodiment 1 ~ embodiment 3 and comparative example 1 ~ 3 obtain is injection molded into and detects batten accordingly, the Performance Detection of constant temperature (23 DEG C ± 2 DEG C), the laggard line correlation of constant humidity (50% ± 5%) 24h, detects data as shown in table 1 below:
Table 1 Halogen low-poison and combustion-resisting strengthens the performance detection data of PBT composite (15% glass)
Embodiment 4
As one embodiment of the present of invention, the preparation method of described PBT mold composition comprises the following steps:
(1) get the raw materials ready according to following component and content: limiting viscosity is the PBT resin 4990g of 0.95dl/g, diethyl hypo-aluminum orthophosphate 1450g, hexaphenoxycyclotriphosphazene 250g, ethylene methyl methacrylate-glycidyl acrylate 250g, filament diameter are 11um the alkali free glass fibre 3000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Embodiment 5
As one embodiment of the present of invention, the preparation method of described PBT mold composition comprises the following steps:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 5090g, the melamine polyphosphate 1480g of 0.95dl/g, six ethoxy basic ring three phosphonitrile 120g, glycidyl methacrylate graft polyoxyethylene 250g, filament diameter are 11um the alkali free glass fibre 3000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Embodiment 6
As one embodiment of the present of invention, the preparation method of described PBT mold composition comprises the following steps:
(1) get the raw materials ready according to following component and content: limiting viscosity is the PBT resin 5000g of 0.95dl/g, diphenyl phosphonic acid aluminium 1510g, hexaphenoxycyclotriphosphazene 180g, ethylene methyl methacrylate-glycidyl acrylate 250g, filament diameter are 11um the alkali free glass fibre 3000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Comparative example 4:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 4990g, the diethyl hypo-aluminum orthophosphate 1700g of 0.95dl/g, ethylene methyl methacrylate-glycidyl acrylate 250g, filament diameter are 11um the alkali free glass fibre 3000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Comparative example 5:
(1) get the raw materials ready according to following component and content: limiting viscosity is the PBT resin 4990g of 0.95dl/g, diethyl hypo-aluminum orthophosphate 1650g, phenoxy cyclotriphosphazene 50g, ethylene methyl methacrylate-glycidyl acrylate 250g, filament diameter are 11um the alkali free glass fibre 3000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Comparative example 6:
(1) get the raw materials ready according to following component and content: limiting viscosity is the PBT resin 4990g of 0.95dl/g, diethyl hypo-aluminum orthophosphate 1150g, phenoxy cyclotriphosphazene 650g, ethylene methyl methacrylate-glycidyl acrylate 250g, filament diameter are 11um the alkali free glass fibre 3000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
The Halogen low-poison and combustion-resisting PBT reinforced composite that embodiment 4 ~ embodiment 6 and comparative example 4 ~ 6 obtain is injection molded into and detects batten accordingly, the Performance Detection of constant temperature (23 DEG C ± 2 DEG C), the laggard line correlation of constant humidity (50% ± 5%) 24h, detects data as shown in table 2 below:
Table 2 Halogen low-poison and combustion-resisting strengthens the performance detection data of PBT composite (30% glass)
Embodiment 7
As one embodiment of the present of invention, the preparation method of described PBT mold composition comprises the following steps:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 4280g, the aluminum diethylphosphinate 1250g of 0.84dl/g, six ethoxy basic ring three phosphonitrile 190g, glycidyl methacrylate graft polyoxyethylene 220g, filament diameter are 10um the alkali free glass fibre 4000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Embodiment 8
As one embodiment of the present of invention, the preparation method of described PBT mold composition comprises the following steps:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 4280g, the diphenyl phosphonic acid aluminium 1220g of 0.84dl/g, six ethoxy basic ring three phosphonitrile 220g, glycidyl methacrylate graft polyoxyethylene 220g, filament diameter are 10um the alkali free glass fibre 4000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Embodiment 9
As one embodiment of the present of invention, the preparation method of described PBT mold composition comprises the following steps:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 4280g, the melamine polyphosphate 1220g of 0.84dl/g, hexaphenoxycyclotriphosphazene 240g, glycidyl methacrylate graft polyoxyethylene 220g, filament diameter are 10um the alkali free glass fibre 4000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Comparative example 7:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 4280g, the aluminum diethylphosphinate 1440g of 0.84dl/g, ethylene methyl methacrylate-glycidyl acrylate 250g, filament diameter are 13um the alkali free glass fibre 3000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Comparative example 8:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 4290g, the aluminum diethylphosphinate 1405g of 0.84dl/g, hexaphenoxycyclotriphosphazene 35g, ethylene methyl methacrylate-glycidyl acrylate 250g, filament diameter are 13um the alkali free glass fibre 4000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
Comparative example 9:
(1) get the raw materials ready according to following component and content: limiting viscosity is PBT resin 4280g, the aluminum diethylphosphinate 940g of 0.84dl/g, six ethoxy basic ring three phosphonitrile 500g, ethylene methyl methacrylate-glycidyl acrylate 250g, filament diameter are 13um the alkali free glass fibre 4000g of surface through silane coupling agent process, oxidation inhibitor B225 30g and lubricant PETS 30g.
(2) with embodiment 1.
The Halogen low-poison and combustion-resisting PBT reinforced composite that embodiment 7 ~ embodiment 9 and comparative example 7 ~ 9 obtain is injection molded into and detects batten accordingly, the Performance Detection of constant temperature (23 DEG C ± 2 DEG C), the laggard line correlation of constant humidity (50% ± 5%) 24h, detects data as shown in table 3 below:
Table 3 Halogen low-poison and combustion-resisting strengthens the performance detection data of PBT composite
Find out from above test data, organophosphorus nitrile compound not only has good cooperative flame retardant effect, when its consumption is 1% ~ 3% time, can also give matrix material good mechanical property.Therefore, halogen-free flame-retardant glass fiber of the present invention strengthens PBT material not only good, the smokeless low toxicity of flame retardant properties, meets European Union environmental protection requirement, and its mechanical property has reached or close to the suitable level of the PBT bromine antimony fire retardant material of current main flow.
The present invention aims to provide a kind ofly to be had excellent thermostability and flame retardant properties, not to discharge toxic substance, environmental friendliness, and the high halogen-free flame-retardant glass fiber of mechanical property strengthens PBT moulding compound.In the present invention, after the organophosphorus nitrile compound of interpolation 1% ~ 3%, the mechanical property of the discovery moulding compound that contriver is surprised obtains significant raising, and continues the consumption strengthening organic phosphonitrile, and the mechanical property of moulding compound but starts obvious decline.Visible, the special construction of organophosphorus nitrile compound significantly improves organic secondary phosphine acid salt and trimeric cyanamide polyphosphonic acid and receives the consistency of halogen-free flame retardants system and PBT resin, and the mechanical property of moulding compound is improved.But when addition continues to increase, the more embodiments of organophosphorus nitrile compound be flame retardant properties, and due to the plastification of organophosphorus nitrile compound, cause moulding compound mechanical property to decline.
The invention has the beneficial effects as follows:
(1) PBT moulding compound of the present invention is not halogen-containing, and excellent fireproof performance;
(2) from the viewpoint of environmental protection, PBT moulding compound of the present invention produces without toxic substance in high temperature process or when storing, and meets European Union environmental protection requirement completely;
(3) PBT moulding compound mechanical property of the present invention is high, close to the level that the PBT bromine antimony fire retardant material of current main flow is suitable;
(4) moulding compound preparation method of the present invention is simple, high machinery performance halogen-free low-poison and combustion-resisting fiber glass reinforced PBT moulding compound is prepared by each component being used for PBT moulding compound mutually being mixed, conventional dry blend melting granulating technology can be adopted, without any special restriction.
Those of ordinary skill in the field are to be understood that: the discussion of above any embodiment is only exemplary, and not intended to be implies that the scope of the present disclosure (comprising claim) is limited to these examples; Under thinking of the present invention, also can combine between technical characteristic in above embodiment or different embodiment, step can realize with random order, and there are other changes many of different aspect of the present invention as above, and they do not provide in details for the sake of simplicity.Therefore, within the spirit and principles in the present invention all, any omission made, amendment, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a PBT mold composition, is characterized in that, its composition comprises by massfraction:
PBT 30％～70％；
Halogen-free flame retardants 12% ~ 20%;
Organophosphorus nitrile compound 1% ~ 3%;
Toughner 0% ~ 5%;
Glass fibre 10% ~ 40%.
2. PBT mold composition according to claim 1, is characterized in that, described organophosphorus nitrile compound is selected from least one in six ethoxy basic ring three phosphonitriles and hexaphenoxycyclotriphosphazene.
3. PBT mold composition according to claim 1, it is characterized in that, described halogen-free flame retardants is selected from least one in organic secondary phosphine acid salt and melamine polyphosphate.
4. PBT mold composition according to claim 3, is characterized in that, described organic secondary phosphine acid salt is selected from least one in aluminum diethylphosphinate and diphenyl phosphonic acid aluminium.
5. PBT mold composition according to claim 1, is characterized in that, the limiting viscosity of described PBT is 0.7 ~ 1.1dl/g.
6. PBT mold composition according to claim 1, is characterized in that, described toughner is selected from least one in ethylene methyl methacrylate-glycidyl acrylate, glycidyl methacrylate graft polyoxyethylene.
7. PBT mold composition according to claim 1, is characterized in that, described glass fibre is the alkali free glass fibre of filament diameter 10um ~ 13um.
8. PBT mold composition according to claim 1, is characterized in that, the surface of described glass fibre is through silane coupling agent process.
9. PBT mold composition according to claim 1, is characterized in that, described PBT mold composition also comprises: oxidation inhibitor B225 and lubricant PETS, and the quality sum of described oxidation inhibitor B225 and lubricant PETS accounts for 0 ~ 2% of described PBT mold composition.
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| CN106751558A (en) * | 2016-11-18 | 2017-05-31 | 无锡明盛纺织机械有限公司 | A kind of engineering plastic materials and preparation method containing bamboo fibre |
| CN113372715A (en) * | 2021-06-23 | 2021-09-10 | 杭州本松新材料技术股份有限公司 | Red phosphorus flame-retardant reinforced nylon composite material and application thereof |
| CN117551338A (en) * | 2024-01-12 | 2024-02-13 | 北京慕湖新材料技术有限公司 | Flame-retardant cold-resistant and damp-heat-resistant polyester composition and preparation method thereof |
| KR102656925B1 (en) * | 2023-12-08 | 2024-04-17 | 주식회사 코솔러스 | Phosphorous flame-retardant compound and method for manufacturing the same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106751558A (en) * | 2016-11-18 | 2017-05-31 | 无锡明盛纺织机械有限公司 | A kind of engineering plastic materials and preparation method containing bamboo fibre |
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| KR102656925B1 (en) * | 2023-12-08 | 2024-04-17 | 주식회사 코솔러스 | Phosphorous flame-retardant compound and method for manufacturing the same |
| CN117551338A (en) * | 2024-01-12 | 2024-02-13 | 北京慕湖新材料技术有限公司 | Flame-retardant cold-resistant and damp-heat-resistant polyester composition and preparation method thereof |
| CN117551338B (en) * | 2024-01-12 | 2024-03-26 | 北京慕湖新材料技术有限公司 | Flame-retardant cold-resistant and damp-heat-resistant polyester composition and preparation method thereof |
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Application publication date: 20150930 |