CN107163518A - It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite and preparation method thereof - Google Patents
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite and preparation method thereof Download PDFInfo
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- CN107163518A CN107163518A CN201710493328.5A CN201710493328A CN107163518A CN 107163518 A CN107163518 A CN 107163518A CN 201710493328 A CN201710493328 A CN 201710493328A CN 107163518 A CN107163518 A CN 107163518A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/003—Additives being defined by their diameter
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The present invention relates to technical field of polymer materials, specifically related to it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite and preparation method thereof, this can the high glowing filament ignition temperature flame-retardant PBT composite of laser marking include the raw material of following parts by weight：40 60 parts of PBT resin, 25 35 parts of glass fibre, 10 15 parts of main flame retardant, 5 10 parts of synergistic flame retardant of compounding, 26 parts of toughener, 0.5 1.0 parts of laser marking powder, 0.1 0.2 parts of antioxidant, 0.5 1.0 parts of other auxiliary agents.The present invention can the high glowing filament ignition temperature flame-retardant PBT composite of laser marking can both meet high glowing filament ignition temperature, laser marking, and good flame retardation effect are can be used for again, resistance to gentle weather resistance is excellent, and intensity is high, excellent shock resistance, processing characteristics is excellent, excellent combination property.
Description
Technical field
The present invention relates to technical field of polymer materials, and in particular to it is a kind of can laser marking high glowing filament ignition temperature
Anti-flaming PBT composite and preparation method thereof.
Background technology
PBT be it is a kind of it is translucent arrive opaque creamy white crystals thermoplastic polyester, be five large-engineering plastics it is important into
One of member.It has excellent mechanical performance, electrical property, heat resistance, wearability, chemical resistance, formability and good size
Stability, is widely used in the fields such as electronic apparatus, automobile, machinery.
Due to PBT These characteristics, flame-retardant PBT is widely used in the field of electronics such as capacitor, relay.With
The development of science and technology and stepping up for living standards of the people, household self energyization will be realized gradually, uncared for electrical equipment when using
Equipment also will be increasing, therefore the company such as beautiful, Gree proposes the electronic apparatus plastic part used household electrical appliance successively
Meet the requirement of high glowing filament ignition temperature.
Other aspects, with continuing to develop for the new material relevant industries such as automobile, machinery, electrical equipment, the use to material
New requirement is constantly proposed, lightweight, high-performance, environmental protection become new trend, and substantial amounts of metal material is by engineering plastics
Replaced, PBT accounts for critically important status as representative therein.Further, people also propose more to engineering material
It is high, more specifically require：Such as, people have more pursuits for the color of product, and this requires engineering material to have
The advantage of easy dyeing；People are based on needing product identification, false proof etc., it is desirable to which engineering material can carry out laser marking.
Furthermore, existing PBT material weatherability is poor, therefore, and high glowing filament ignition temperature can be met by developing one kind
It can be used for laser marking again and the PBT composite with high-weatherability be particularly important.
The content of the invention
, can laser marking it is an object of the invention to provide one kind in order to overcome shortcoming and defect present in prior art
High glowing filament ignition temperature flame-retardant PBT composite, the PBT composite can both meet high glowing filament ignition temperature, again
It can be used for laser marking, and good flame retardation effect, resistance to gentle weather resistance is excellent, intensity is high, excellent shock resistance, processability
Can excellent, excellent combination property.
Another object of the present invention is to provide it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite woods
The preparation method of material, the preparation method step is simple, convenient operation and control, steady quality, and production efficiency is high, and production cost is low,
Can large-scale industrial production.
The purpose of the present invention is achieved through the following technical solutions：It is a kind of can laser marking high glowing filament ignition temperature flame-retardant
PBT composite, the PBT composite includes the raw material of following parts by weight：
40-60 parts of PBT resin
25-35 parts of glass fibre
10-15 parts of main flame retardant
Compound 5-10 parts of synergistic flame retardant
2-6 parts of toughener
0.5-1.0 parts of laser marking powder
0.1-0.2 parts of antioxidant
Other auxiliary agent 0.5-1.0 parts.
The present invention can laser marking high glowing filament ignition temperature flame-retardant PBT composite by using above-mentioned raw materials,
And the weight proportion of each raw material is strictly controlled, obtained PBT composite can both meet high glowing filament ignition temperature, again can be with
For laser marking, and good flame retardation effect, resistance to gentle weather resistance is excellent, and intensity is high, and excellent shock resistance, processing characteristics is excellent
It is good, excellent combination property.
It is preferred that, the PBT resin is polybutylene terephthalate (PBT) of the inherent viscosity in 0.7-1.2dL/g.
Polybutylene terephthalate (PBT) of the invention by using above-mentioned inherent viscosity is as PBT resin, obtained PBT
Composite has excellent mechanical performance, electrical property, heat resistance, wearability, chemical resistance, formability and good size steady
It is qualitative.
It is preferred that, the glass fibre is the chopped glass of alkali-free that filament diameter is handled on 10-15 μm and surface through silane coupler
Glass fiber.
The alkali-free short glass fiber that the present invention is handled by using above-mentioned filament diameter and surface through silane coupler, system
The PBT composite tensile strength obtained is high, and electrical insulating property is good, and heatproof is high, and non-ignitable, anti-corruption, heat-insulated, sound-proofing is good.
It is preferred that, the main flame retardant is that brominated Polystyrene, the poly- carbon of bromination and mean molecule quantity are 10000-50000's
At least one of brominated epoxy resin.It is more highly preferred to, the main flame retardant is by brominated Polystyrene, the poly- carbon peace of bromination
Average molecular weight compares 1.5-2.5 for 10000-50000 brominated epoxy resin with weight:0.5-1.5:The mixture of 1 composition.
The present invention can reach good flame retardant effect, moreover it is possible to improve the processing of material by using above-mentioned main flame retardant
Performance and mechanical performance.
It is preferred that, the compounding synergistic flame retardant is antimony oxide, sodium antimonate, melamine cyanurate, hypophosphorous acid
At least two in aluminium and melamine polyphosphate.Be more highly preferred to, it is described compounding synergistic flame retardant be by antimony oxide,
Sodium antimonate and melamine polyphosphate are with weight ratio 1:0.8-1.2:1.4-2.2 the mixture of composition.
The present invention is by using above-mentioned compounding synergistic flame retardant, and main flame retardant compounding use, with synergistic effect, can be with
Improve the flame retardant effect of material, moreover it is possible to improve the processing characteristics and mechanical performance of material.
It is preferred that, the toughener is by ethylene-methyl acrylate-glycidyl acrylate and ethylene-acrylic acid fourth
Ester compares 0.8-1.2 with weight：The mixture of 1 composition.
The present invention strictly controls its weight proportion by using above-mentioned toughener, can improve the tough of PBT composite
Property and mechanical and physical performance.
It is preferred that, the laser marking powder is at least one of tin-oxide, sb oxide and neodymium oxides.It is more excellent
Choosing, the laser marking powder is with weight to compare 0.5-1.5 by tin-oxide, sb oxide and neodymium oxides:1:2-4 compositions
Mixture.
The present invention is by using above-mentioned laser marking powder so that PBT composite is easier by laser marking, is greatly improved
The definition of PBT composite laser-marking.
It is preferred that, the antioxidant is with weight to compare 1-2 by antioxidant 1010 and irgasfos 168:The mixture of 1 composition.
Species, compounding and weight proportion of the invention by strictly controlling antioxidant, can delay or suppress material oxidation
The progress of process, so as to prevent the aging of material and extend its service life.
It is preferred that, other auxiliary agents are toner.The toner is titanium dioxide of the particle diameter at 1-5 μm；The titanium dioxide is
By rutile type titanium white and anatase thpe white powder with weight ratio 1：1.5-2.5 the mixture of composition.
The present invention using particle diameter in 1-5 μm of titanium dioxide as toner, further using rutile type titanium white and rutile titania
Type titanium dioxide compounding use, and control its weight ratio to be 1：1.5-2.5, with superior whiteness, tinting strength, tinting power, covering power, weather-proof
Property, heat resistance and chemical stability, particularly no toxicity.
The PBT composite also includes 0.8-1.2 parts of 0.5-1.5 parts of anti-dripping agent and lubricant.
The anti-dripping agent is that polytetrafluoroethylene (PTFE), MMA coating modifications PTFE and AS coating modification PTFE compare 1-2 with weight:
0.8-1.2:The mixture of 1 composition.Polytetrafluoroethylene (PTFE), English abbreviation is PTFE, and MMA full name is methyl methacrylate, AS
Full name be acrylonitritrile-styrene resin.
The flame-retardant anti-dropping effect for the polytetrafluoroethylene (PTFE) not coated is preferable, but poor with polyester compatibility, can be certain
The polytetrafluoroethylene (PTFE) of the mechanical property of material, MMA claddings or AS claddings is influenceed in degree, its flame-retardant anti-dropping effect is somewhat poor
A bit, but the loss of material mechanical performance can be made up.
The present invention is used as anti-dripping agent by using polytetrafluoroethylene (PTFE), MMA coating modification PTFE and AS coating modifications PTFE
Compounding use, and its weight proportion is strictly controlled, obtained polyester composite anti-dripping effects is good, improves integral material
Compatibility, it is ensured that the excellent properties of material property.
The lubricant is with weight ratio by OPE, pentaerythritol stearate and ethylene bis stearic acid amide
1.5-2.5：1：The mixture of 0.8-1.2 compositions.
The present invention, as external lubricant, can reduce PBT melts and mould, the friction of machine barrel using OPE；Adopt
With pentaerythritol stearate and ethylene bis stearic acid amide as in-lubricant, the intermolecular friction of PBT melts can be reduced；Three
Plant lubricant and 1.5-2.5 is compared with weight：1：0.8-1.2 compounding uses can make material improve the flowing of material in process
The release property of property and product.
In order to further enhance the intensity and mechanical property of PBT composite, the PBT composite also includes aliphatic
15-35 parts of polyketone.
The present invention, can be with PBT formation alloy materials, Ke Yiti by adding aliphatic polyketone in PBT composite
The intensity and shock resistance of high PBT composite, also with excellent wearability, chemical resistance, fuel resistance and hydrolysis
Property.
In order to further enhance the mechanical property and processing characteristics of PBT composite, the PBT composite also includes expanding
0.001-0.005 parts of 0.001-0.005 parts of chain agent and end-capping reagent.
The present invention strictly controls its consumption by using chain extender, can be with the functional group on linear polymer PBT chains
React and extend strand, molecular weight increase, so as to strengthen the mechanical property and processing characteristics of PBT composite.It is preferred that,
The chain extender is pyromellitic acid dianhydride, poly- benzo-dioxazole, bis-epoxy bisphenol-A-diglycidyl ether, 4,4'- diphenylmethyls
At least one of alkane diisocyanate and triphenyl phosphite.Be more highly preferred to, the chain extender be by pyromellitic acid dianhydride,
Bis-epoxy bisphenol-A-diglycidyl ether and 4,4'- methyl diphenylene diisocyanate compare 0.8-1.2 with weight:1.4-2.2:1
The mixture of composition.
The present invention strictly controls its consumption by using end-capping reagent, in advance carries out PBT ends-OH bases and end-COOH bases
Toughener containing active function groups, can be fixed in PBT phases, reach and PBT is entered by reaction end-blocking by the bonding that chemically reacts
The effect of row toughness reinforcing, so as to greatly improve the impact flexibility of alloy material.It is preferred that, the end-capping reagent is MBS, ABS, EMA-g-
At least one of GMA, EMA-g-MAH and ACR toughener grafting active function groups；Wherein, the active function groups include anti-
Butene dioic acid, maleic anhydride, glycidyl acrylate or epoxy resin.Be more highly preferred to, the end-capping reagent be by MBS,
EMA-g-GMA and ACR toughener Graft Epoxy Resin is with weight ratio 1:0.5-1.5:1.5-2.5 the mixture of composition.
Another object of the present invention is achieved through the following technical solutions：It is a kind of can laser marking high glowing filament ignition temperature
The preparation method of anti-flaming PBT composite, comprises the following steps：
（1）The various raw materials in addition to glass fibre are weighed by weight；
（2）The PBT resin weighed up is first premixed into 1.5-2.5min, then the original weighed up with other with diffusing oil in high-speed mixer
Material is mixed after 1.5-2.5min and discharged again, through double screw extruder extruding pelletization, and glass fibre claims to add by side feeding through weightlessness,
Be made can laser marking high glowing filament ignition temperature flame-retardant PBT composite；
Wherein, the double screw extruder each section of processing temperature since feeding section is respectively：170-190℃、190-210
℃、190-210℃、200-220℃、200-220℃、200-220℃、210-230℃、210-230℃、210-230℃、220-
240 DEG C, head temperature is 230-250 DEG C, and screw speed is 320-400r/min.
The beneficial effects of the present invention are：The present invention can laser marking high glowing filament ignition temperature flame-retardant PBT be combined
Material can both meet high glowing filament ignition temperature, and laser marking, and good flame retardation effect, resistance to gentle weather resistance are can be used for again
Excellent, intensity is high, and excellent shock resistance, processing characteristics is excellent, excellent combination property.
The preparation method step of the present invention is simple, convenient operation and control, steady quality, and production efficiency is high, and production cost is low,
Can large-scale industrial production.
Embodiment
For the ease of the understanding of those skilled in the art, with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying is referred to not limitation of the invention.
Embodiment 1
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, the PBT composite includes following weight
Measure the raw material of part：
40 parts of PBT resin
25 parts of glass fibre
10 parts of main flame retardant
Compound 5 parts of synergistic flame retardant
2 parts of toughener
0.5 part of laser marking powder
0.1 part of antioxidant
Other 0.5 part of auxiliary agents.
The PBT resin is polybutylene terephthalate (PBT) of the inherent viscosity in 0.7dL/g.
The glass fibre is the alkali-free short glass fiber that filament diameter is handled on 10 μm and surface through silane coupler.
The main flame retardant is brominated Polystyrene.
The compounding synergistic flame retardant is antimony oxide and sodium antimonate with weight ratio 1:The mixture of 1 composition.
The toughener is with weight by ethylene-methyl acrylate-glycidyl acrylate and Ethylene-butyl acrylate
Than 0.8：The mixture of 1 composition.
The laser marking powder is tin-oxide.
The antioxidant is with weight ratio 1 by antioxidant 1010 and irgasfos 168:The mixture of 1 composition.
Other auxiliary agents are toner.
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite preparation method, including following step
Suddenly：
（1）The various raw materials in addition to glass fibre are weighed by weight；
（2）The PBT resin weighed up is first premixed into 1.5min with diffusing oil in high-speed mixer, then the raw material weighed up with other is again
Discharged after mixed 1.5min, through double screw extruder extruding pelletization, glass fibre claims to add by side feeding through weightlessness, and being made to swash
The high glowing filament ignition temperature flame-retardant PBT composite of light mark；
Wherein, the double screw extruder each section of processing temperature since feeding section is respectively：170℃、190℃、190℃、
200 DEG C, 200 DEG C, 200 DEG C, 210 DEG C, 210 DEG C, 210 DEG C, 220 DEG C, head temperature is 230 DEG C, and screw speed is 320r/min.
Embodiment 2
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, the PBT composite includes following weight
Measure the raw material of part：
45 parts of PBT resin
28 parts of glass fibre
11 parts of main flame retardant
Compound 6 parts of synergistic flame retardant
3 parts of toughener
0.6 part of laser marking powder
0.12 part of antioxidant
Other 0.6 part of auxiliary agents.
The PBT resin is polybutylene terephthalate (PBT) of the inherent viscosity in 0.8dL/g.
The glass fibre is the alkali-free short glass fiber that filament diameter is handled on 11 μm and surface through silane coupler.
The main flame retardant is the poly- carbon of bromination.
The compounding synergistic flame retardant is antimony oxide and melamine cyanurate with weight ratio 1:The mixing of 1 composition
Thing.
The toughener is with weight by ethylene-methyl acrylate-glycidyl acrylate and Ethylene-butyl acrylate
Than 0.9：The mixture of 1 composition.
The laser marking powder is sb oxide.
The antioxidant is with weight ratio 1.2 by antioxidant 1010 and irgasfos 168:The mixture of 1 composition.
Other auxiliary agents are toner.
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite preparation method, including following step
Suddenly：
（1）The various raw materials in addition to glass fibre are weighed by weight；
（2）The PBT resin weighed up is first premixed into 1.8min with diffusing oil in high-speed mixer, then the raw material weighed up with other is again
Discharged after mixed 1.8min, through double screw extruder extruding pelletization, glass fibre claims to add by side feeding through weightlessness, and being made to swash
The high glowing filament ignition temperature flame-retardant PBT composite of light mark；
Wherein, the double screw extruder each section of processing temperature since feeding section is respectively：175℃、195℃、195℃、
205 DEG C, 205 DEG C, 205 DEG C, 215 DEG C, 215 DEG C, 215 DEG C, 225 DEG C, head temperature is 235 DEG C, and screw speed is 340r/min.
Embodiment 3
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, the PBT composite includes following weight
Measure the raw material of part：
50 parts of PBT resin
30 parts of glass fibre
12 parts of main flame retardant
Compound 8 parts of synergistic flame retardant
4 parts of toughener
0.8 part of laser marking powder
0.15 part of antioxidant
Other 0.8 part of auxiliary agents.
The PBT resin is polybutylene terephthalate (PBT) of the inherent viscosity in 0.9dL/g.
The glass fibre is the alkali-free short glass fiber that filament diameter is handled on 12 μm and surface through silane coupler.
The main flame retardant is the brominated epoxy resin that mean molecule quantity is 10000.
The compounding synergistic flame retardant is antimony oxide and hypo-aluminum orthophosphate with weight ratio 1:The mixture of 1 composition.
The toughener is with weight by ethylene-methyl acrylate-glycidyl acrylate and Ethylene-butyl acrylate
Than 1：The mixture of 1 composition.
The laser marking powder is neodymium oxides.
The antioxidant is with weight ratio 1.5 by antioxidant 1010 and irgasfos 168:The mixture of 1 composition.
Other auxiliary agents are toner.
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite preparation method, including following step
Suddenly：
（1）The various raw materials in addition to glass fibre are weighed by weight；
（2）The PBT resin weighed up is first premixed into 2min with diffusing oil in high-speed mixer, then the raw material weighed up with other is mixed again
Discharged after 2min, through double screw extruder extruding pelletization, glass fibre claims to add by side feeding through weightlessness, be made can laser beat
Target high glowing filament ignition temperature flame-retardant PBT composite；
Wherein, the double screw extruder each section of processing temperature since feeding section is respectively：180℃、200℃、200℃、
210 DEG C, 210 DEG C, 210 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 230 DEG C, head temperature is 240 DEG C, and screw speed is 360r/min.
Embodiment 4
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, the PBT composite includes following weight
Measure the raw material of part：
55 parts of PBT resin
32 parts of glass fibre
14 parts of main flame retardant
Compound 9 parts of synergistic flame retardant
5 parts of toughener
0.9 part of laser marking powder
0.18 part of antioxidant
Other 0.9 part of auxiliary agents.
The PBT resin is polybutylene terephthalate (PBT) of the inherent viscosity in 1.1dL/g.
The glass fibre is the alkali-free short glass fiber that filament diameter is handled on 14 μm and surface through silane coupler.
The main flame retardant is the brominated epoxy resin that mean molecule quantity is 30000.
The compounding synergistic flame retardant is antimony oxide and melamine polyphosphate with weight ratio 1:The mixing of 1 composition
Thing.
The toughener is with weight by ethylene-methyl acrylate-glycidyl acrylate and Ethylene-butyl acrylate
Than 1.1：The mixture of 1 composition.
The laser marking powder is tin-oxide.
The antioxidant is with weight ratio 1.8 by antioxidant 1010 and irgasfos 168:The mixture of 1 composition.
Other auxiliary agents are toner.
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite preparation method, including following step
Suddenly：
（1）The various raw materials in addition to glass fibre are weighed by weight；
（2）The PBT resin weighed up is first premixed into 2.2min with diffusing oil in high-speed mixer, then the raw material weighed up with other is again
Discharged after mixed 2.2min, through double screw extruder extruding pelletization, glass fibre claims to add by side feeding through weightlessness, and being made to swash
The high glowing filament ignition temperature flame-retardant PBT composite of light mark；
Wherein, the double screw extruder each section of processing temperature since feeding section is respectively：185℃、205℃、205℃、
215 DEG C, 215 DEG C, 215 DEG C, 225 DEG C, 225 DEG C, 225 DEG C, 235 DEG C, head temperature is 245 DEG C, and screw speed is 380r/min.
Embodiment 5
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, the PBT composite includes following weight
Measure the raw material of part：
60 parts of PBT resin
35 parts of glass fibre
15 parts of main flame retardant
Compound 10 parts of synergistic flame retardant
6 parts of toughener
1.0 parts of laser marking powder
0.2 part of antioxidant
Other 1.0 parts of auxiliary agents.
The PBT resin is polybutylene terephthalate (PBT) of the inherent viscosity in 1.2dL/g.
The glass fibre is the alkali-free short glass fiber that filament diameter is handled on 15 μm and surface through silane coupler.
The main flame retardant is the brominated epoxy resin that mean molecule quantity is 50000.
The compounding synergistic flame retardant is sodium antimonate, melamine cyanurate, hypo-aluminum orthophosphate and melamine polyphosphoric acid
Salt compares 1 with weight:1:1:The mixture of 1 composition.
The toughener is with weight by ethylene-methyl acrylate-glycidyl acrylate and Ethylene-butyl acrylate
Than 1.2：The mixture of 1 composition.
The laser marking powder is any two kinds in tin-oxide, sb oxide and neodymium oxides with weight ratio 1:1 group
Into mixture.
The laser marking powder is sb oxide.
The antioxidant is with weight ratio 2 by antioxidant 1010 and irgasfos 168:The mixture of 1 composition.
Other auxiliary agents are toner.
It is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite preparation method, including following step
Suddenly：
（1）The various raw materials in addition to glass fibre are weighed by weight；
（2）The PBT resin weighed up is first premixed into 2.5min with diffusing oil in high-speed mixer, then the raw material weighed up with other is again
Discharged after mixed 2.5min, through double screw extruder extruding pelletization, glass fibre claims to add by side feeding through weightlessness, and being made to swash
The high glowing filament ignition temperature flame-retardant PBT composite of light mark；
Wherein, the double screw extruder each section of processing temperature since feeding section is respectively：190℃、210℃、210℃、
220 DEG C, 220 DEG C, 220 DEG C, 230 DEG C, 230 DEG C, 230 DEG C, 240 DEG C, head temperature is 250 DEG C, and screw speed is 400r/min.
Embodiment 6
The difference of the present embodiment and above-described embodiment 1 is：
The main flame retardant be by brominated Polystyrene, the poly- carbon of bromination and mean molecule quantity for 10000 brominated epoxy resin with
Weight compares 1.5:0.5:The mixture of 1 composition.
The compounding synergistic flame retardant is with weight ratio 1 by antimony oxide, sodium antimonate and melamine polyphosphate:
0.8:The mixture of 1.4 compositions.
The laser marking powder is with weight ratio 0.5 by tin-oxide, sb oxide and neodymium oxides:1:2 compositions it is mixed
Compound.
The toner is titanium dioxide of the particle diameter at 1 μm；The titanium dioxide is by rutile type titanium white and anatase titanium dioxide
Powder compares 1 with weight：The mixture of 1.5 compositions.
The PBT composite also includes 0.8 part of 0.5 part of anti-dripping agent and lubricant.
The anti-dripping agent is polytetrafluoroethylene (PTFE), MMA coating modifications PTFE and AS coating modification PTFE with weight ratio 1:
0.8:The mixture of 1 composition.
The lubricant is with weight ratio by OPE, pentaerythritol stearate and ethylene bis stearic acid amide
1.5：1：The mixture of 0.8 composition.
The PBT composite also includes 15 parts of aliphatic polyketone.
The PBT composite also includes 0.001 part of 0.001 part of chain extender and end-capping reagent.
The chain extender is by pyromellitic acid dianhydride, bis-epoxy bisphenol-A-diglycidyl ether and 4,4'- diphenyl methane
Diisocyanate compares 0.8 with weight:1.4:The mixture of 1 composition.
The end-capping reagent is with weight ratio 1 by MBS, EMA-g-GMA and ACR toughener Graft Epoxy Resin:0.5:1.5 group
Into mixture.
Embodiment 7
The difference of the present embodiment and above-described embodiment 2 is：
The main flame retardant be by brominated Polystyrene, the poly- carbon of bromination and mean molecule quantity for 20000 brominated epoxy resin with
Weight compares 1.8:0.8:The mixture of 1 composition.
The compounding synergistic flame retardant is with weight ratio 1 by antimony oxide, sodium antimonate and melamine polyphosphate:
0.9:The mixture of 1.6 compositions.
The laser marking powder is with weight ratio 0.8 by tin-oxide, sb oxide and neodymium oxides:1:2.5 compositions
Mixture.
The toner is titanium dioxide of the particle diameter at 2 μm；The titanium dioxide is by rutile type titanium white and anatase titanium dioxide
Powder compares 1 with weight：The mixture of 1.8 compositions.
The PBT composite also includes 0.9 part of 0.8 part of anti-dripping agent and lubricant.
The anti-dripping agent is polytetrafluoroethylene (PTFE), MMA coating modifications PTFE and AS coating modification PTFE with weight ratio 1.2:
0.9:The mixture of 1 composition.
The lubricant is with weight ratio by OPE, pentaerythritol stearate and ethylene bis stearic acid amide
1.8：1：The mixture of 0.9 composition.
The PBT composite also includes 20 parts of aliphatic polyketone.
The PBT composite also includes 0.002 part of 0.002 part of chain extender and end-capping reagent.
The chain extender is by pyromellitic acid dianhydride, bis-epoxy bisphenol-A-diglycidyl ether and 4,4'- diphenyl methane
Diisocyanate compares 0.9 with weight:1.6:The mixture of 1 composition.
The end-capping reagent is with weight ratio 1 by MBS, EMA-g-GMA and ACR toughener Graft Epoxy Resin:0.8:1.8 group
Into mixture.
Embodiment 8
The difference of the present embodiment and above-described embodiment 3 is：
The main flame retardant be by brominated Polystyrene, the poly- carbon of bromination and mean molecule quantity for 30000 brominated epoxy resin with
Weight compares 2:1:The mixture of 1 composition.
The compounding synergistic flame retardant is with weight ratio 1 by antimony oxide, sodium antimonate and melamine polyphosphate:1:
The mixture of 1.8 compositions.
The laser marking powder is with weight ratio 1 by tin-oxide, sb oxide and neodymium oxides:1:The mixing of 3 compositions
Thing.
The toner is titanium dioxide of the particle diameter at 3 μm；The titanium dioxide is by rutile type titanium white and anatase titanium dioxide
Powder compares 1 with weight：The mixture of 2 compositions.
The PBT composite also includes 1 part of 1 part of anti-dripping agent and lubricant.
The anti-dripping agent is polytetrafluoroethylene (PTFE), MMA coating modifications PTFE and AS coating modification PTFE with weight ratio 1.5:
1:The mixture of 1 composition.
The lubricant is with weight ratio by OPE, pentaerythritol stearate and ethylene bis stearic acid amide
2：1：The mixture of 1 composition.
The PBT composite also includes 25 parts of aliphatic polyketone.
The PBT composite also includes 0.003 part of 0.003 part of chain extender and end-capping reagent.
The chain extender is by pyromellitic acid dianhydride, bis-epoxy bisphenol-A-diglycidyl ether and 4,4'- diphenyl methane
Diisocyanate compares 1 with weight:1.8:The mixture of 1 composition.
The end-capping reagent is with weight ratio 1 by MBS, EMA-g-GMA and ACR toughener Graft Epoxy Resin:1:2 compositions
Mixture.
Embodiment 9
The difference of the present embodiment and above-described embodiment 4 is：
The main flame retardant be by brominated Polystyrene, the poly- carbon of bromination and mean molecule quantity for 40000 brominated epoxy resin with
Weight compares 2.2:1.2:The mixture of 1 composition.
The compounding synergistic flame retardant is with weight ratio 1 by antimony oxide, sodium antimonate and melamine polyphosphate:
1.1:The mixture of 2 compositions.
The laser marking powder is with weight ratio 1.2 by tin-oxide, sb oxide and neodymium oxides:1:3.5 compositions
Mixture.
The toner is titanium dioxide of the particle diameter at 4 μm；The titanium dioxide is by rutile type titanium white and anatase titanium dioxide
Powder compares 1 with weight：The mixture of 2.2 compositions.
The PBT composite also includes 1.1 parts of 1.2 parts of anti-dripping agent and lubricant.
The anti-dripping agent is polytetrafluoroethylene (PTFE), MMA coating modifications PTFE and AS coating modification PTFE with weight ratio 1.8:
1.1:The mixture of 1 composition.
The lubricant is with weight ratio by OPE, pentaerythritol stearate and ethylene bis stearic acid amide
2.2：1：The mixture of 1.1 compositions.
The PBT composite also includes 30 parts of aliphatic polyketone.
The PBT composite also includes 0.004 part of 0.004 part of chain extender and end-capping reagent.
The chain extender is by pyromellitic acid dianhydride, bis-epoxy bisphenol-A-diglycidyl ether and 4,4'- diphenyl methane
Diisocyanate compares 1.1 with weight:2:The mixture of 1 composition.
The end-capping reagent is with weight ratio 1 by MBS, EMA-g-GMA and ACR toughener Graft Epoxy Resin:1.2:2.2 group
Into mixture.
Embodiment 10
The difference of the present embodiment and above-described embodiment 5 is：
The main flame retardant be by brominated Polystyrene, the poly- carbon of bromination and mean molecule quantity for 50000 brominated epoxy resin with
Weight compares 2.5:1.5:The mixture of 1 composition.
The compounding synergistic flame retardant is with weight ratio 1 by antimony oxide, sodium antimonate and melamine polyphosphate:
1.2:The mixture of 2.2 compositions.
The laser marking powder is with weight ratio 1.5 by tin-oxide, sb oxide and neodymium oxides:1:4 compositions it is mixed
Compound.
The toner is titanium dioxide of the particle diameter at 5 μm；The titanium dioxide is by rutile type titanium white and anatase titanium dioxide
Powder compares 1 with weight：The mixture of 2.5 compositions.
The PBT composite also includes 1.2 parts of 1.5 parts of anti-dripping agent and lubricant.
The anti-dripping agent is polytetrafluoroethylene (PTFE), MMA coating modifications PTFE and AS coating modification PTFE with weight ratio 2:
1.2:The mixture of 1 composition.
The lubricant is with weight ratio by OPE, pentaerythritol stearate and ethylene bis stearic acid amide
2.5：1：The mixture of 1.2 compositions.
The PBT composite also includes 35 parts of aliphatic polyketone.
The PBT composite also includes 0.005 part of 0.005 part of chain extender and end-capping reagent.
The chain extender is by pyromellitic acid dianhydride, bis-epoxy bisphenol-A-diglycidyl ether and 4,4'- diphenyl methane
Diisocyanate compares 1.2 with weight:2.2:The mixture of 1 composition.
The end-capping reagent is with weight ratio 1 by MBS, EMA-g-GMA and ACR toughener Graft Epoxy Resin:1.5:2.5 group
Into mixture.
The present invention can the high glowing filament ignition temperature flame-retardant PBT composite of laser marking entered according to GB/T 5169.13
Row test, its GWIT can reach more than 850 DEG C, can meet high glowing filament ignition temperature, and laser marking is can be used for again, and
Anti-flammability can reach V0 grades of UL94（0.8mm）, good flame retardation effect, hot and humid（As temperature be 85 DEG C, humidity be 85% wet
Degree）Under the conditions of experiment can mistake 168h, resistance to gentle weather resistance is excellent, and tensile strength can reach more than 125Mpa, bending strength
More than 185Mpa can be reached, intensity is high, and notch impact strength can reach 11Kj/m2More than, excellent shock resistance, processing
Function admirable, excellent combination property.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with other manner,
Any obvious replacement is within protection scope of the present invention on the premise of not departing from present inventive concept.
Claims (10)
1. it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, it is characterised in that：The PBT is combined
Material includes the raw material of following parts by weight：
40-60 parts of PBT resin
25-35 parts of glass fibre
10-15 parts of main flame retardant
Compound 5-10 parts of synergistic flame retardant
2-6 parts of toughener
0.5-1.0 parts of laser marking powder
0.1-0.2 parts of antioxidant
Other auxiliary agent 0.5-1.0 parts.
2. it is according to claim 1 it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, it is special
Levy and be：The PBT resin is polybutylene terephthalate (PBT) of the inherent viscosity in 0.7-1.2dL/g.
3. it is according to claim 1 it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, it is special
Levy and be：The glass fibre is that filament diameter is fine in the alkali-free staple glass that 10-15 μm and surface are handled through silane coupler
Dimension.
4. it is according to claim 1 it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, it is special
Levy and be：The main flame retardant is the brominated epoxy that brominated Polystyrene, the poly- carbon of bromination and mean molecule quantity are 10000-50000
At least one of resin.
5. it is according to claim 1 it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, it is special
Levy and be：The compounding synergistic flame retardant is antimony oxide, sodium antimonate, melamine cyanurate, hypo-aluminum orthophosphate and trimerization
At least two in cyanamide Quadrafos.
6. it is according to claim 1 it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, it is special
Levy and be：The toughener is with weight by ethylene-methyl acrylate-glycidyl acrylate and Ethylene-butyl acrylate
Compare 0.8-1.2：The mixture of 1 composition.
7. it is according to claim 1 it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, it is special
Levy and be：The laser marking powder is at least one of tin-oxide, sb oxide and neodymium oxides.
8. it is according to claim 1 it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, it is special
Levy and be：The antioxidant is with weight to compare 1-2 by antioxidant 1010 and irgasfos 168:The mixture of 1 composition.
9. it is according to claim 1 it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite, it is special
Levy and be：Other auxiliary agents are toner.
10. as described in claim any one of 1-9 it is a kind of can laser marking high glowing filament ignition temperature flame-retardant PBT composite woods
The preparation method of material, it is characterised in that：Comprise the following steps：
（1）The various raw materials in addition to glass fibre are weighed by weight；
（2）The PBT resin weighed up is first premixed into 1.5-2.5min, then the original weighed up with other with diffusing oil in high-speed mixer
Material is mixed after 1.5-2.5min and discharged again, through double screw extruder extruding pelletization, and glass fibre claims to add by side feeding through weightlessness,
Be made can laser marking high glowing filament ignition temperature flame-retardant PBT composite；
Wherein, the double screw extruder each section of processing temperature since feeding section is respectively：170-190℃、190-210
℃、190-210℃、200-220℃、200-220℃、200-220℃、210-230℃、210-230℃、210-230℃、220-
240 DEG C, head temperature is 230-250 DEG C, and screw speed is 320-400r/min.
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| WO2018073819A1 (en) * | 2016-10-18 | 2018-04-26 | Bromine Compounds Ltd. | Flame-retarded polyester formulations |
| CN109929225A (en) * | 2019-03-25 | 2019-06-25 | 广东顺德顺炎新材料股份有限公司 | A kind of laser indigo plant is cracked down evil force flame-retardant PBT material and preparation method thereof |
| CN110023389A (en) * | 2016-11-30 | 2019-07-16 | 帝斯曼知识产权资产管理有限公司 | Thermoplastic compounds |
| CN110240786A (en) * | 2019-05-08 | 2019-09-17 | 南通开普乐工程塑料有限公司 | A kind of PBT composite and preparation method thereof with good laser mark performance |
| CN113105727A (en) * | 2021-04-13 | 2021-07-13 | 东莞市东翔塑胶有限公司 | Weather-resistant high-glow-wire polyester composite material and preparation method thereof |
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| CN102952379A (en) * | 2012-12-04 | 2013-03-06 | 上海日之升新技术发展有限公司 | Environment-friendly flame retardant glass fiber reinforced polybutylece terephthalate (PBT) material with high comparative tracking index (CTI) value and high glow wire ignition temperature (GWIT) value and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018073819A1 (en) * | 2016-10-18 | 2018-04-26 | Bromine Compounds Ltd. | Flame-retarded polyester formulations |
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