CN102108190A - Green flame-retarding reinforced polybutylene terephthalate composition and preparation method thereof - Google Patents
Green flame-retarding reinforced polybutylene terephthalate composition and preparation method thereof Download PDFInfo
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- CN102108190A CN102108190A CN2009102472966A CN200910247296A CN102108190A CN 102108190 A CN102108190 A CN 102108190A CN 2009102472966 A CN2009102472966 A CN 2009102472966A CN 200910247296 A CN200910247296 A CN 200910247296A CN 102108190 A CN102108190 A CN 102108190A
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Abstract
The invention relates to a green flame-retarding reinforced polybutylene terephthalate composition and a preparation method thereof. The composition comprises the following components in percentage by weight: 30 to 70 percent of polybutylene terephthalate (PBT) resin, 5 to 50 percent of alkali-free glass fibers, 0.1 to 18 percent of flame retardant A, 0.1 to 20 percent of flame retardant B, 1 to 20 percent of toughening agent, 0.1 to 1 percent of lubricating agent, and 0.1 to 1 percent of antioxygen. After the PBT resin is dried, other components excluding the glass fibers are filled into a high-speed mixer in a ratio to be mixed; the mixture and the glass fibers then are extruded and granulated in a screw extruder; and under the conveying and shearing actions of the double-screw extruder, the product is obtained by melt plasticizing, kneading, blending, extruding at machine head, bracing, cooling, granulating, and drying. Compared with the prior art, the composition belongs to a green flame-retarding product and has high flame-retarding effect, the added toughening agent improves the toughness of the material, and the preparation method is simple in operation.
Description
Technical field
The present invention relates to a kind of polymeric composition and preparation method thereof, especially relate to a kind of environmental protection flame retardant enhancement type polybutylene terephthalate composition and preparation method.
Background technology
In recent years, flame-retardant PBT demand in electronic apparatus and each industrial circle is increasing, its performance characteristics is: shaping speed is fast, flame retardant properties is good, chemical proofing etc., and glass fibre enhancing PBT material not only has excellent physical and mechanical properties such as physical strength height, resistance to fatigue and dimensional stabilizing are good, creep properties is little, ageing-resistant performance excellence, and its electrical property is also very excellent, as its volume specific resistance and dielectric strength height, arc resistance can be excellent, stable performance under wet environment.Because the electronic apparatus part all has fire-retardant requirement in various degree, it is necessary therefore using flame-retardant reinforced PBT in these fields.
Traditional flame-retardant PBT employing bromide fire retardant and antimonous oxide are composite, this flame-retardant system can produce a large amount of smog and discharge deleterious corrosive hydrogen halides gas when burning, in the face of more and more stricter environmental requirement, the research of environmental protection flame retardant material has been obtained the great attention of various countries, and the market requirement of product is also more urgent.Environment-friendly flame retardant PBT mainly adopts red phosphorus to do fire retardant at present, and there is following shortcoming in it, and the one, this series products can only be black or redness, can't produce other color; The 2nd, this series products smell when injection moulding is bigger, the red phosphorus dieseling can occur when injection moulding speed and pressure are big, has separating out of a little phosphorus on the mould during long-time injection moulding; The 3rd, the red phosphorus flame-retardant product is placed on for a long time that the surface has the globule in the higher environment of humidity, and under higher envrionment temperature, mechanics attenuation ratio bromo-ether flame retardant products is fast.
The brominated triazine fire retardant is different from the bromo-ether based flame retardant, it is the collaborative environment friendly flame retardant of a kind of bromine nitrogen, the flame retarding efficiency height, Heat stability is good, not volatile separating out, outward appearance is pure white, anti-ultraviolet radiation and photostabilization excellence, be specially adapted to have ABS, PC/ABS alloy, plastics such as HIPS, PBT than high processing temperature, little Huang or Vandyke brown fire retardants such as alternative bromination epoxy, brominated Polystyrene satisfy that product is fire-retardant, the composite request of outward appearance and other performances.Phosphate flame retardants and brominated triazine fire retardant is composite, can produce the flame retardant effect of phosphorus-nitrogen-triple synergistics of bromine.
Summary of the invention
Purpose of the present invention is exactly environmental protection flame retardant enhancement type polybutylene terephthalate composition and the preparation method who provides a kind of Heat stability is good for the defective that overcomes above-mentioned prior art existence, can produce multiple color.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of environmental protection flame retardant enhancement type polybutylene terephthalate composition is characterized in that, said composition comprises following component and content (wt%):
Polybutylene terephthalate (PBT) resin 30-70;
Alkali free glass fibre 5-50;
Fire retardant A 0.1-18;
Fire retardant B 0.1-20;
Toughner 1-20;
Lubricant 0.1-1;
Oxidation inhibitor 0.1-1.
Described alkali free glass fibre is the alkali free glass fibre through coupling agent treatment, and described coupling agent comprises commercially available silane coupling agent KH550.
Described fire retardant A is the brominated triazine compound.
Described fire retardant B is a phosphate compounds, comprises ammonium polyphosphate, melamine pyrophosphate.
Described toughner comprises one or more in ethylene-methyl methacrylate butyl ester-glycidyl acrylate terpolymer, ethylene-methyl acrylate copolymer or the ethylene-vinyl acetate copolymer copolymer.
Described lubricant comprises that OP is cured, lipid acid or stearate.
Described oxidation inhibitor is that Hinered phenols antioxidant or Hinered phenols antioxidant and phosphite ester kind antioxidant are 1: 1 compound by weight, described Hinered phenols antioxidant comprises commercially available antioxidant 1076, oxidation inhibitor 245 or antioxidant 1010, and described phosphite ester kind antioxidant comprises commercially available oxidation inhibitor 168.
A kind of environmental protection flame retardant enhancement type polybutylene terephthalate preparation of compositions method is characterized in that this method may further comprise the steps:
(1) prepare raw material according to following component and content (wt%):
Polybutylene terephthalate (PBT) resin 30-70,
Alkali free glass fibre 5-50,
Fire retardant A 0.1-18,
Fire retardant B 0.1-20,
Toughner 1-20,
Lubricant 0.1-1,
Oxidation inhibitor 0.1-1;
(2) PBT resin dry 4-6h under 120-140 ℃, to except that glass fibre, other component put into high-speed mixer mixing 2-5min in proportion, reinstate the screw extrusion press extruding pelletization with glass fibre one then, the control screw speed is 250-350rpm, under the conveying and shearing action of twin screw extruder, through fusion plastification, kneading is mixing, head is extruded, tie rod, cooling, pelletizing, drying, promptly obtains product.
Described twin screw extruder from the charging opening to the head each section extruder temperature be respectively 220 ℃, 230 ℃, 240 ℃, 250 ℃, 240 ℃, 230 ℃, 230 ℃, 220 ℃, 220 ℃.
Compared with prior art, the present invention has the following advantages:
(1) the present invention is composite as fire retardant with brominated triazine and phosphate compounds, and the PBT material of production belongs to the environmental protection flame retardant product, has good flame-retardant effect.When the fire retardant consumption is 18%, the alkali free glass fibre consumption is 30% o'clock, can reach 1.6mm vertical combustion V-0; When the fire retardant consumption is 30%, the alkali free glass fibre consumption is 20% o'clock, can reach 0.8mm vertical combustion V-0;
(2) improved the toughness of material by adding toughner, product easy dyeing of the present invention has abundant colors;
(3) preparation method of the present invention is simple to operate.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
Environment-friendly flame-retardant reinforced PBT prescription (weight percentage):
PBT resin: 47%, alkali free glass fibre: 30%, fire retardant A is the brominated triazine compound: 12%, fire retardant B is an ammonium polyphosphate: 6%, toughner is ethylene-methyl methacrylate butyl ester-glycidyl acrylate terpolymer: 5%, lubricant is an OP wax: 0.3%, and oxidation inhibitor is 1076/1010 (weight ratio is 1: 1): 0.4%.
The PBT resin is dry 5h under 130 ℃, to except that glass fibre, other component put into high-speed mixer mixing 5min in proportion, reinstate the screw extrusion press extruding pelletization with glass fibre one then, the control screw speed is 300rpm, under the conveying and shearing action of twin screw extruder, through fusion plastification, kneading is mixing, head is extruded, tie rod, cooling, pelletizing, drying, promptly obtains product.Twin screw extruder from the charging opening to the head each section extruder temperature be respectively 220 ℃, 230 ℃, 240 ℃, 250 ℃, 240 ℃, 230 ℃, 230 ℃, 220 ℃, 220 ℃.
Embodiment 2
Environment-friendly flame-retardant reinforced PBT prescription (weight percentage):
PBT resin: 45%, alkali free glass fibre: 20%, fire retardant A is the brominated triazine compound: 18%, fire retardant B is a melamine pyrophosphate: 12%, toughner is ethylene-methyl methacrylate butyl ester-glycidyl acrylate terpolymer: 5%, lubricant is a calcium stearate: 0.3%, and oxidation inhibitor is 245/1010 (weight ratio is 1: 1): 0.4%.
The PBT resin is dry 4h under 140 ℃, to except that glass fibre, other component put into high-speed mixer mixing 2min in proportion, reinstate the screw extrusion press extruding pelletization with glass fibre one then, the control screw speed is 250rpm, under the conveying and shearing action of twin screw extruder, through fusion plastification, kneading is mixing, head is extruded, tie rod, cooling, pelletizing, drying, promptly obtains product.Twin screw extruder from the charging opening to the head each section extruder temperature be respectively 220 ℃, 230 ℃, 240 ℃, 250 ℃, 240 ℃, 230 ℃, 230 ℃, 220 ℃, 220 ℃.
Embodiment 3
Environment-friendly flame-retardant reinforced PBT prescription (weight percentage):
PBT resin: 45%, alkali free glass fibre: 20%, fire retardant A is the brominated triazine compound: 24%, fire retardant B is the melamine pyrophosphate compound: 6%, toughner is the ethylene-methyl acrylate copolymer: 5%, lubricant is a calcium stearate: 0.3%, and oxidation inhibitor is 245/1010 (weight ratio is 1: 1): 0.4%.
The PBT resin is dry 6h under 120 ℃, to except that glass fibre, other component put into high-speed mixer mixing 5min in proportion, reinstate the screw extrusion press extruding pelletization with glass fibre one then, the control screw speed is 350rpm, under the conveying and shearing action of twin screw extruder, through fusion plastification, kneading is mixing, head is extruded, tie rod, cooling, pelletizing, drying, promptly obtains product.Twin screw extruder from the charging opening to the head each section extruder temperature be respectively 220 ℃, 230 ℃, 240 ℃, 250 ℃, 240 ℃, 230 ℃, 230 ℃, 220 ℃, 220 ℃.
Embodiment 4
Environment-friendly flame-retardant reinforced PBT prescription (weight percentage):
PBT resin: 47%, alkali free glass fibre: 30%, fire retardant A is the brominated triazine compound: 4%, fire retardant B is an ammonium polyphosphate: 14%, toughner is the compound (weight ratio is 1: 1) of ethylene-methyl acrylate copolymer, ethylene-vinyl acetate copolymer copolymer: 5%, lubricant is a calcium stearate: 0.3%, and oxidation inhibitor is 245/1010 (weight ratio is 1: 1): 0.4%.
The PBT resin is dry 5h under 120 ℃, to except that glass fibre, other component put into high-speed mixer mixing 3min in proportion, reinstate the screw extrusion press extruding pelletization with glass fibre one then, the control screw speed is 280rpm, under the conveying and shearing action of twin screw extruder, through fusion plastification, kneading is mixing, head is extruded, tie rod, cooling, pelletizing, drying, promptly obtains product.Twin screw extruder from the charging opening to the head each section extruder temperature be respectively 220 ℃, 230 ℃, 240 ℃, 250 ℃, 240 ℃, 230 ℃, 230 ℃, 220 ℃, 220 ℃.
Embodiment 5
A kind of environmental protection flame retardant enhancement type polybutylene terephthalate preparation of compositions method, this method may further comprise the steps:
(1) prepare raw material according to following component and content:
PBT resin 30kg, alkali free glass fibre 50kg, this alkali free glass fibre is through silane coupling agent KH550 processing, brominated triazine compound 18kg, ammonium polyphosphate compound 0.1kg, ethylene-methyl methacrylate butyl ester-glycidyl acrylate terpolymer 1kg, the cured 0.1kg of OP, oxidation inhibitor 2450.1kg;
(2) PBT resin dry 6h under 130 ℃, to except that glass fibre, other component put into high-speed mixer mixing 5min in proportion, reinstate the screw extrusion press extruding pelletization with glass fibre one then, the control screw speed is 300rpm, under the conveying and shearing action of twin screw extruder, through fusion plastification, kneading is mixing, head is extruded, tie rod, cooling, pelletizing, drying, promptly obtains product.Twin screw extruder from the charging opening to the head each section extruder temperature be respectively 220 ℃, 230 ℃, 240 ℃, 250 ℃, 240 ℃, 230 ℃, 230 ℃, 220 ℃, 220 ℃.
Embodiment 6
A kind of environmental protection flame retardant enhancement type polybutylene terephthalate preparation of compositions method, this method may further comprise the steps:
(1) prepare raw material according to following component and content:
PBT resin 70kg, alkali free glass fibre 5kg, this alkali free glass fibre is through silane coupling agent KH550 processing, brominated triazine compound 0.1kg, melamine pyrophosphate 20kg, ethylene-vinyl acetate copolymer copolymer 5kg, sodium stearate 0.1kg, oxidation inhibitor 168 0.2kg;
(2) PBT resin dry 5h under 120 ℃, to except that glass fibre, other component put into high-speed mixer mixing 5min in proportion, reinstate the screw extrusion press extruding pelletization with glass fibre one then, the control screw speed is 350rpm, under the conveying and shearing action of twin screw extruder, through fusion plastification, kneading is mixing, head is extruded, tie rod, cooling, pelletizing, drying, promptly obtains product.Twin screw extruder from the charging opening to the head each section extruder temperature be respectively 220 ℃, 230 ℃, 240 ℃, 250 ℃, 240 ℃, 230 ℃, 230 ℃, 220 ℃, 220 ℃.
Embodiment 1～6 resulting environment-friendly flame-retardant reinforced PBT composition product is compared with currently available products, has higher mechanical property, and tensile strength can reach 115MPa, and flexural strength can reach 170MPa, and the socle girder notched Izod impact strength can reach 9KJ/m
2Good heat resistance, heat-drawn wire (1.82MPa) can reach 210 ℃; 1.6mm vertical combustion can reach V-0.
Claims (9)
1. an environmental protection flame retardant enhancement type polybutylene terephthalate composition is characterized in that, said composition comprises following component and content (wt%):
Polybutylene terephthalate (PBT) resin 30-70;
Alkali free glass fibre 5-50;
Fire retardant A 0.1-18;
Fire retardant B 0.1-20;
Toughner 1-20;
Lubricant 0.1-1;
Oxidation inhibitor 0.1-1.
2. a kind of environmental protection flame retardant enhancement type polybutylene terephthalate composition according to claim 1, it is characterized in that, described alkali free glass fibre is the alkali free glass fibre through coupling agent treatment, and described coupling agent comprises commercially available silane coupling agent KH550.
3. a kind of environmental protection flame retardant enhancement type polybutylene terephthalate composition according to claim 1 is characterized in that described fire retardant A is the brominated triazine compound.
4. a kind of environmental protection flame retardant enhancement type polybutylene terephthalate composition according to claim 1 is characterized in that described fire retardant B is a phosphate compounds, comprises ammonium polyphosphate, melamine pyrophosphate.
5. a kind of environmental protection flame retardant enhancement type polybutylene terephthalate composition according to claim 1, it is characterized in that described toughner comprises one or more in ethylene-methyl methacrylate butyl ester-glycidyl acrylate terpolymer, ethylene-methyl acrylate copolymer or the ethylene-vinyl acetate copolymer copolymer.
6. a kind of environmental protection flame retardant enhancement type polybutylene terephthalate composition according to claim 1 is characterized in that, described lubricant comprises that OP is cured, lipid acid or stearate.
7. a kind of environmental protection flame retardant enhancement type polybutylene terephthalate composition according to claim 1, it is characterized in that, described oxidation inhibitor is that Hinered phenols antioxidant or Hinered phenols antioxidant and phosphite ester kind antioxidant are 1: 1 compound by weight, described Hinered phenols antioxidant comprises commercially available antioxidant 1076, oxidation inhibitor 245 or antioxidant 1010, and described phosphite ester kind antioxidant comprises commercially available oxidation inhibitor 168.
8. environmental protection flame retardant enhancement type polybutylene terephthalate preparation of compositions method is characterized in that this method may further comprise the steps:
(1) prepare raw material according to following component and content (wt%):
Polybutylene terephthalate (PBT) resin 30-70,
Alkali free glass fibre 5-50,
Fire retardant A 0.1-18,
Fire retardant B 0.1-20,
Toughner 1-20,
Lubricant 0.1-1,
Oxidation inhibitor 0.1-1;
(2) PBT resin dry 4-6h under 120-140 ℃, to except that glass fibre, other component put into high-speed mixer mixing 2-5min in proportion, reinstate the screw extrusion press extruding pelletization with glass fibre one then, the control screw speed is 250-350rpm, under the conveying and shearing action of twin screw extruder, through fusion plastification, kneading is mixing, head is extruded, tie rod, cooling, pelletizing, drying, promptly obtains product.
9. a kind of environmental protection flame retardant enhancement type polybutylene terephthalate preparation of compositions method according to claim 8, it is characterized in that, described twin screw extruder from the charging opening to the head each section extruder temperature be respectively 220 ℃, 230 ℃, 240 ℃, 250 ℃, 240 ℃, 230 ℃, 230 ℃, 220 ℃, 220 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321349A (en) * | 2011-08-05 | 2012-01-18 | 江阴市龙山合成材料有限公司 | Fiber glass reinforced halogen-free flame retardant PBT |
| CN108624008A (en) * | 2018-04-24 | 2018-10-09 | 嘉兴希卡姆复合材料有限公司 | A kind of flame-retardant enhanced PBT material and preparation method thereof |
-
2009
- 2009-12-28 CN CN2009102472966A patent/CN102108190A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102321349A (en) * | 2011-08-05 | 2012-01-18 | 江阴市龙山合成材料有限公司 | Fiber glass reinforced halogen-free flame retardant PBT |
| CN102321349B (en) * | 2011-08-05 | 2012-10-03 | 江阴市龙山合成材料有限公司 | Glass fiber reinforced halogen-free flame-retardant polybutylene terephthalate (PBT) |
| CN108624008A (en) * | 2018-04-24 | 2018-10-09 | 嘉兴希卡姆复合材料有限公司 | A kind of flame-retardant enhanced PBT material and preparation method thereof |
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Application publication date: 20110629 |