CN104725797B - Method for preparing flame-retardant plastic composite material - Google Patents

Method for preparing flame-retardant plastic composite material Download PDF

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CN104725797B
CN104725797B CN201510141837.2A CN201510141837A CN104725797B CN 104725797 B CN104725797 B CN 104725797B CN 201510141837 A CN201510141837 A CN 201510141837A CN 104725797 B CN104725797 B CN 104725797B
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composite
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pbt
flame
flame retardant
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CN104725797A (en
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杨明山
赵祎宁
李长峰
向攀
杨朝金
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Crystallization Engineering Plastics Co Ltd Of Foshan City
Beijing Institute of Petrochemical Technology
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Crystallization Engineering Plastics Co Ltd Of Foshan City
Beijing Institute of Petrochemical Technology
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Abstract

The invention discloses a method for preparing a flame-retardant plastic composite material. The method comprises the following steps: firstly drying polybutylene terephthalate (PBT) in an air dry oven at 110-120 DEG C for 4-6 hours, and drying acrylonitrile-butadiene-styrene copolymer (ABS) in the air dry oven at 60-70 DEG C for 2-4 hours; weighing corresponding raw materials according to the set mass percentage, and mixing the weighed raw materials into a high-speed mixer; adding the mixture into a twin-screw extruder for melting and mixing, cooling in a water tank, and granulating in a granulator to obtain the flame-retardant plastic composite material. The composite material prepared by the method has relatively high impact toughness, excellent processing performance and excellent flame retardant performance, and can be applied to the fields of automobiles, household appliances, electronic information and the like.

Description

A kind of preparation method of flame retardant plastics composite
Technical field
The present invention relates to engineering plastic alloy technical field, more particularly, to a kind of preparation side of flame retardant plastics composite Method.
Background technology
In recent years, plastics industry has obtained significant progress, and wherein engineering plastics particularly abs is in electrical equipment, traffic, calculating The fields such as machine have obtained specification application.Abs is the maximum engineering plastics of consumption, and it is acrylonitrile-butadiene-styrene (ABS) copolymerization Thing, has the characteristics such as good fluidity, high mechanical properties, surface quality be good, but abs be readily burned in itself, not ageing-resistant (variable Yellow), also limit its application the shortcomings of heat resistance is low, price is high.Traditional fire-retardant abs is to compound using brominated flame-retardant to contain antimony Compound, however, bromide can produce toxic gas during burning, and antimony oxide is also toxic, to health Cause negative effect with environment.
In order to realize the environmental protection halogen-free flameproof of abs, many researchers have been carried out studying, and mainly pass through hydroxide (as aluminium hydroxide, magnesium hydroxide) or phosphonium flame retardant (as red phosphorus and phosphate etc.) replace bromide and antimony oxide.But The flame retardant effect of hydroxide is poor, needs addition big, therewith the process flowability decline bringing abs and mechanical property deterioration Cannot use.And nitrogenous, phosphorus flame-retardant system is as a kind of new Green Flammability system, there is higher flame retarding efficiency, be Replace the main trend of bromine-containing compound at present.In addition, pbt (polybutylene terephthalate (PBT)) have high heat-resisting, high intensity, The good characteristic of resistance to ag(e)ing, and price is relatively low, is also the wide engineering plastics of application, but its toughness is poor, processing fluidity Bad, surface property is bad, and due to pbt and abs poor compatibility, simple blend poor performance, particularly impact flexibility is low, therefore Need increase-volume and toughness reinforcing.
Fire-retardant pbt/abs alloy material of the prior art, or not being halogen-free environment-friendly flame-proof, or be impact flexibility relatively Low, or being that mobility is bad, range of application is not extensive.
Content of the invention
It is an object of the invention to provide a kind of preparation method of flame retardant plastics composite, by answering prepared by the method Condensation material has higher impact flexibility and good process industrial art performance, has excellent fire resistance simultaneously, can automobile, Use in the fields such as household electrical appliances, electronic information.
A kind of preparation method of flame retardant plastics composite, methods described includes:
First polybutylene terephthalate (PBT) pbt is dried 4~6 hours in the air dry oven at 110~120 DEG C, And acrylonitrile-butadiene-styrene copolymer abs is dried 2~4 hours in the air dry oven at 60~70 DEG C;
Weigh corresponding raw material according still further to the mass percent setting, and the raw material being weighed are added to mixed at a high speed Mixed in conjunction machine;Wherein, each constituent mass percentage of described raw material is: 30~50% pbt, 20~35% Abs, 1~5% compound compatilizer, 1~5% composite toughing agent, 10~30% composite flame-retardant agent, 0.5~2% compound Lubricant, 0.3~0.6% composite antioxidant, 0.1~1% silicone oil, 0.1~1% polytetrafluoroethylene (PTFE) and 0.1~ 0.5% Ethyltriphenylphosphonium brimide;
Add mixture to again and in double screw extruder, carry out melting mixing, tank cooling and pelleter pelletizing operation, Obtain described flame retardant plastics composite.
As seen from the above technical solution provided by the invention, had by the composite prepared by the method higher Impact flexibility and good process industrial art performance, there is excellent fire resistance simultaneously, can be in automobile, household electrical appliances, electronic information Use Deng in field.
Brief description
In order to be illustrated more clearly that the technical scheme of the embodiment of the present invention, below will be to required use in embodiment description Accompanying drawing be briefly described it should be apparent that, drawings in the following description are only some embodiments of the present invention, for this For the those of ordinary skill in field, on the premise of not paying creative work, other can also be obtained according to these accompanying drawings Accompanying drawing.
Fig. 1 is the preparation method schematic flow sheet of the embodiment of the present invention provided flame retardant plastics composite;
The structural representation of the double screw extruder that Fig. 2 is provided by the embodiment of the present invention.
Specific embodiment
With reference to the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Ground description is it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on this Inventive embodiment, the every other enforcement that those of ordinary skill in the art are obtained under the premise of not making creative work Example, broadly falls into protection scope of the present invention.
Embodiment of the present invention methods described uses phosphonium flame retardant, and with the novel elastomer containing a large amount of nitrogens-poly- Phosphonitrile combine, compounding linear phenolic resin as the flame-retardant additive of pbt/abs, be equipped with compound compatilizer, composite toughing agent and The components such as compounded lubricant, the flame retardant plastics composite of preparation environmental protection, so that fire resistance is greatly improved, have high simultaneously Mobility and high toughness, can be used for household electrical appliances, automobile, electronics, electrically and the field such as information products.Below in conjunction with accompanying drawing to this Inventive embodiments are described in further detail, and are illustrated in figure 1 the embodiment of the present invention provided flame retardant plastics composite Preparation method schematic flow sheet, described preparation method includes:
Step 11: first by polybutylene terephthalate (PBT) pbt in the air dry oven at 110~120 DEG C be dried 4~ 6 hours, and it is little acrylonitrile-butadiene-styrene copolymer abs to be dried in the air dry oven at 60~70 DEG C 2~4 When;
In implementing, the intrinsic viscosity of adopted pbt is 0.75~0.95dl/g.Here intrinsic viscosity is molecular weight Sign, pbt molecular weight is too low, and the impact flexibility of alloy is low;Conversely, pbt molecular weight is too high, the poor fluidity of alloy.
Adopted abs be high impact grade, melt index (mi) between 1~5g/10min (200 DEG C, 5kgf), high-impact Abs and pbt blending can obtain the high engineering plastic alloy of impact flexibility.
Step 12: weigh corresponding raw material according still further to the mass percent setting, and the raw material being weighed are added Mixed in high-speed mixer;
In this step, specifically can be with mixed at high speed 1 minute.Each constituent mass percentage of above-mentioned raw material is: 30~ The compound compatilizer of 50% pbt, 20~35% abs, 1~5%, 1~5% composite toughing agent, 10~30% compound Fire retardant, 0.5~2% compounded lubricant, 0.3~0.6% composite antioxidant, 0.1~1% silicone oil, 0.1~1% Polytetrafluoroethylene (PTFE) and 0.1~0.5% Ethyltriphenylphosphonium brimide;
In implementing, the compound compatilizer being adopted is styrene-maleic anhydride copolymer sma, ethylene acrylic Acrylate copolymer ptw and styrene-acrylonitrile-GMA terpolymer sag is according to the quality of 1:1:1 Than mixed mixture.Here, from also having shock resistance in 40 degrees below zero, material is pliable and tough, can be used as toughener for ptw; Eba polarity is high simultaneously, and various polymer compatibility is good, raising fire retardant is also had with the interfacial adhesion of abs, pbt simultaneously Facilitation.Epoxide group on sag can react with the end carboxyl of pbt, thus playing compatibilization.Three compounds has association Same effect.
The composite toughing agent being adopted is high glue powder, has the MBS of core shell structure Copolymer mbs and ethylene vinyl acetate copolymer eva is according to the mixed mixture of mass ratio of 1:1:1;Wherein, described height Butadiene content in rubber powder is 40~60wt%, and the va content in described eva is 22~30wt%.Here, high glue powder is permissible It is considered the high abs powder of rubber content, good with abs compatibility, toughening effect projects.Mbs has core shell structure, and shell is first Base acrylic acid esters co-polymer, good with pbt, abs compatibility, core is the higher BS of rubber content, increases Tough excellent effect.The existing good toughening effect of eva is it is also possible to carry heavy alloyed processing fluidity.Three compound have collaborative Effect.
The composite flame-retardant agent being adopted is ethyl hypo-aluminum orthophosphate, Firebrake ZB, linear phenolic resin (75~90 DEG C of softening point) With polyphenylene oxide phosphonitrile (number-average molecular weight is more than 40000) according to 2:1:1:0.5 the mixed mixture of mass ratio.This In, ethyl hypo-aluminum orthophosphate is new halogen-free phosphorus-containing fire retardant agent, particularly has excellent flame retardant effect to polyester (pbt etc.); Firebrake ZB also has smoke suppressing effect;Linear phenolic resin can improve charring rate, thus having flame retardant effect;Big due to the addition of The fire retardant of amount, the impact toughness decreased of composite, not only pairing gold utensil has excellent anti-flammability to polyphosphazene elastomer, also has There is excellent toughening effect, toughening effect is good.Therefore, composite flame-retardant agent is that phosphorus-nitrogen is combined, and charring rate height, smoke-suppressing are good simultaneously, There is cooperative effect.
The compounded lubricant being adopted is ethylene bis stearamide ebs, Brazil wax and OPE are according to 1: The mixed mixture of mass ratio of 1:1.Here, ebs and Brazil wax can increase mobility and surface quality, and oxidation is poly- Ethylene waxes also have the peptizaiton promoting fire retardant, and three compounds has cooperative effect.
The composite antioxidant being adopted is antioxidant tetrapentaerythritol ester (i.e. four [β-(3,5- di-t-butyl -4- hydroxy benzenes Base) propionic acid] pentaerythritol ester) and triphosphite ester (i.e. three [2.4- di-tert-butyl-phenyl] phosphite ester) according to 1:2 quality Than mixed mixture.
The silicone oil being adopted is dimethicone, and viscosity is in 1000~5000mpa.s, preferably 1500~3000mpa.s.This In, due to the addition of substantial amounts of fire retardant, the mobility of composite can receive impact, therefore adds silicone oil to improve composite wood Material process flowability, simultaneously silicone oil there is certain flame retardant effect to abs.
The polytetrafluoroethylene (PTFE) being adopted is powder, and average grain diameter is 3~8 μm.Here add polytetrafluoroethylene (PTFE) can press down System drippage, thus reach ul-94v0 fire-retardant rank.
And adopt the carboxyl reaction that Ethyltriphenylphosphonium brimide can be catalyzed on epoxide group and pbt, thus strengthening sag's Compatibilization effect.
Step 13: add mixture to again carry out in double screw extruder melting mixing, tank cooling and pelleter cut Grain operation, obtains described flame retardant plastics composite.
In this step, described double screw extruder is the parallel co-rotating twin screw extruder of engagement type;
It is illustrated in figure 2 the structural representation of the double screw extruder that the embodiment of the present invention is provided, in Fig. 2: screw rod is long For 36~44, screw combinations are moderate shear rate combinations mode to footpath ratio, and the temperature of double-screw extruding pelletizing is at 180~250 DEG C Between.Here twin-screw prilling temperature should not be too high, and shearing force during mixing granulation can not be too strong, otherwise easily causes abs's Decompose and incipient scorch, so may result in composite jaundice, mechanical property inferior without use value.
Modified by above-mentioned compound compatilizer, composite toughing agent, composite flame-retardant agent and compounded lubricant, prepared Pbt/abs alloy material has high melt flow rate (MFR) and high impact strength, and the combination property of composite greatly improves, The dimensional stability of obtained product increases, and has excellent fire resistance, can be in the fields such as automobile, household electrical appliances, electronic information Use.
For ease of understanding, with reference to being embodied as the implementation process of the present invention is described further, under be classified as this reality Apply the process conditions of middle sample preparation:
Using sz-900/nb injector injection moulding standard specimen, molding technological condition: injection temperature (charge door) 220/ 230/235/230 DEG C (nozzle), injection pressure 30~50mpa, dwell time 8s, cool time 20s.
The formula of this enforcement 1-3 is as shown in table 1 below:
The formula table of 1-3 implemented by table 1
Then according to the preparation method that above-described embodiment is provided, first that pbt is dry in 110~120 DEG C of air dry ovens Dry 4~6 hours, abs is dried 2~4 hours in 60~70 DEG C of air dry ovens;Then weigh each component by formula rate, It is added in high-speed mixer, mixed at high speed 1 minute;Then melting mixing in double screw extruder, water are added mixture to Groove cools down, and pelleter pelletizing obtains described flame retardant plastics composite.
The screw extruder being used be the parallel co-rotating twin screw extruder of engagement type, screw slenderness ratio be 36~ 44, screw combinations are moderate shear rate combinations mode;The temperature of double-screw extruding pelletizing (technique bar between 180~250 DEG C Part is shown in Table 2).
The granulation process parameters of 1-3 implemented by table 2
Then more obtained composite is detected according to following performance test methods:
Tensile strength and elongation at break: carry out according to gb/t 1040-2006 standard.
Bending strength and bending modulus: carry out according to gb/t 9341-2008 standard.
Notched impact properties: carry out according to gb/t1043-2008 standard.
Heat distortion temperature: carry out according to gb/t1634-2004 standard;Maximum deflection direct stress 1.82mpa, programming rate: 2 ℃/min.
Anti-flammability: vertical combustion performance, tested by ul-94 vertical combustion standard, the thick batten thick with 1.6mm of 3.2mm.
Oxygen index (OI) is tested: carries out by gb/t2406-2008 standard.
Molding shrinkage: carry out by gb/t 15585-1995 standard.
The performance implementing the composite obtained by 1-3 is shown in Table 3:
The performance of table 3 composite
As can be seen from the above Table 3, changed by compound compatilizer, composite toughing agent, composite flame-retardant agent and compounded lubricant After property, prepared composite has high melt flow rate (MFR) and high impact strength, and the combination property of composite is big Big raising, the dimensional stability of obtained product increases, and illustrates that compound compatilizer, composite toughing agent and compounded lubricant serve Act on well, can be used for being molded large-scale product, such as electric appliance casing, automobile component etc., overcome fire-retardant pbt/abs in the past and close The bad shortcoming of golden material flowability, has reached halogen-free environment-friendly flame-proof simultaneously, has positive contribution to environmental protection.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto, Any those familiar with the art in the technical scope of present disclosure, the change or replacement that can readily occur in, All should be included within the scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims Enclose and be defined.

Claims (5)

1. a kind of preparation method of flame retardant plastics composite is it is characterised in that methods described includes:
First polybutylene terephthalate (PBT) pbt is dried 4~6 hours in the air dry oven at 110~120 DEG C, and will Acrylonitrile-butadiene-styrene copolymer abs is dried 2~4 hours in the air dry oven at 60~70 DEG C;
Weigh corresponding raw material according still further to the mass percent setting, and the raw material being weighed are added to high-speed mixer In mixed;Wherein, each constituent mass percentage of described raw material is: 30~50% pbt, 20~35% abs, 1 ~5% compound compatilizer, 1~5% composite toughing agent, 10~30% composite flame-retardant agent, 0.5~2% composite lubricated Agent, 0.3~0.6% composite antioxidant, 0.1~1% silicone oil, 0.1~1% polytetrafluoroethylene (PTFE) and 0.1~0.5% Ethyltriphenylphosphonium brimide;
Add mixture to again and in double screw extruder, carry out melting mixing, tank cooling and pelleter pelletizing operation, obtain Described flame retardant plastics composite;
Wherein, the compound compatilizer being adopted is styrene-maleic anhydride copolymer sma, ethylene butyl acrylate copolymer ptw Mixed mixed according to the mass ratio of 1:1:1 with styrene-acrylonitrile-GMA terpolymer sag Compound;
The composite toughing agent being adopted is high glue powder, has the MBS copolymerization of core shell structure Thing mbs and ethylene vinyl acetate copolymer eva is according to the mixed mixture of mass ratio of 1:1:1;Wherein, described high glue powder In butadiene content be 40~60wt%, the va content in described eva be 22~30wt%;
The composite flame-retardant agent being adopted is ethyl hypo-aluminum orthophosphate, Firebrake ZB, linear phenolic resin and polyphenylene oxide phosphonitrile be according to 2: The mixed mixture of mass ratio of 1:1:0.5;
The compounded lubricant being adopted is ethylene bis stearamide ebs, Brazil wax and OPE according to 1:1:1's The mixed mixture of mass ratio;
The composite antioxidant being adopted is antioxidant tetrapentaerythritol ester and triphosphite ester is mixed according to the mass ratio of 1:2 Mixture.
2. according to claim 1 flame retardant plastics composite preparation method it is characterised in that
The intrinsic viscosity of adopted pbt is 0.75~0.95dl/g;Melt index mi of adopted abs 1~5g/10min it Between.
3. according to claim 1 flame retardant plastics composite preparation method it is characterised in that
The silicone oil being adopted is dimethicone, and viscosity is in 1000~5000mpa s.
4. according to claim 1 flame retardant plastics composite preparation method it is characterised in that
The polytetrafluoroethylene (PTFE) being adopted is powder, and average grain diameter is 3~8 μm.
5. according to claim 1 flame retardant plastics composite preparation method it is characterised in that
Described double screw extruder is the parallel co-rotating twin screw extruder of engagement type;
Wherein, screw slenderness ratio is 36~44, and screw combinations are the combination of moderate shear speed, and double-screw extruding pelletizing Temperature between 180~250 DEG C.
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CN105062010B (en) * 2015-07-21 2017-02-08 广州鼎实建筑环保材料有限公司 Flame retardant plastic composite material
CN108329661A (en) * 2017-12-25 2018-07-27 福建华塑新材料有限公司 A kind of flame-retardant reinforced PBT and preparation method thereof applied to electronic apparatus
CN111499791B (en) * 2020-05-13 2021-10-29 佳易容聚合物(上海)有限公司 Application of multi-random copolymer in improving phase structure and phase stability of polyester/styrene resin alloy
CN112724501B (en) * 2020-12-28 2022-03-22 会通新材料股份有限公司 Toughened composite, PBT composite material and preparation method thereof
CN116082784B (en) * 2023-04-10 2023-06-27 佛山市塑聚新材料科技有限公司 Flame-retardant composite material and preparation method and application thereof

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CN101654547A (en) * 2009-09-24 2010-02-24 威海联桥新材料科技股份有限公司 Solid condensation-type organic phosphate flame-retardant PBT/ABS alloy material and preparation method thereof.

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CN103524991A (en) * 2012-07-03 2014-01-22 青岛欣展塑胶有限公司 Halogen-free flame retardant PBT/ABS (polybutylece terephthalate/acrylonitrile butadiene styrene) alloy material and preparation method thereof
CN104277443A (en) * 2014-10-29 2015-01-14 南通日之升高分子新材料科技有限公司 Preparation method of heat-resistant halogen-free flame-retardant PC (polycarbonate)/ABS

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