CN104725797A - Method for preparing flame-retardant plastic composite material - Google Patents

Method for preparing flame-retardant plastic composite material Download PDF

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Publication number
CN104725797A
CN104725797A CN201510141837.2A CN201510141837A CN104725797A CN 104725797 A CN104725797 A CN 104725797A CN 201510141837 A CN201510141837 A CN 201510141837A CN 104725797 A CN104725797 A CN 104725797A
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flame retardant
matrix material
preparation
plastics matrix
retardant plastics
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CN104725797B (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 matrix material
Technical field
The present invention relates to engineering plastic alloy technical field, particularly relate to a kind of preparation method of flame retardant plastics matrix material.
Background technology
In recent years, plastics industry obtains significant progress, wherein engineering plastics particularly ABS obtain Regular application in fields such as electrical equipment, traffic, computers.ABS is the maximum engineering plastics of consumption, it is acrylonitrile-butadiene-styrene copolymer, there is the characteristics such as good fluidity, mechanical property is high, surface quality is good, but ABS itself be easy to burning, not ageing-resistant (easily turn yellow), thermotolerance is low, price is high etc., and shortcoming also limit its application.Traditional flame-proof ABS adopts the composite antimony containing compounds of brominated flame-retardant, but bromide can produce toxic gas between main combustion period, and antimonous oxide is also toxic, causes negative impact to HUMAN HEALTH and environment.
In order to realize the environmental protection halogen-free flameproof of ABS; many investigators are studied, mainly replace bromide and antimonous oxide by oxyhydroxide (as aluminium hydroxide, magnesium hydroxide) or phosphonium flame retardant (as red phosphorus and phosphoric acid salt etc.).But the flame retardant effect of oxyhydroxide is poor, need addition large, worsen thereupon bringing the decline of the process flowability of ABS and mechanical property and cannot use.And the flame-retardant system of nitrogenous, phosphorus is as a kind of novel Green Flammability system, having higher flame retarding efficiency, is the main trend replacing bromine-containing compound at present.In addition, PBT (polybutylene terephthalate) has the characteristic that height is heat-resisting, high strength, ageing resistance are good, and price is lower, be also apply engineering plastics more widely, but its toughness is poor, processing fluidity is bad, surface property is bad, due to PBT and ABS poor compatibility, and simple blend poor performance, particularly impelling strength is low, therefore needs increase-volume and toughness reinforcing.
Flame-retardant PBT/ABS alloy material of the prior art, or be not halogen-free environment-friendly flame-proof, or be that impelling strength is lower, or be that mobility is bad, range of application is not extensive.
Summary of the invention
The object of this invention is to provide a kind of preparation method of flame retardant plastics matrix material, by the matrix material prepared by the method, there is higher impelling strength and good process industrial art performance, there is excellent flame retardant properties simultaneously, can use in the fields such as automobile, household electrical appliances, electronic information.
A preparation method for flame retardant plastics matrix material, described method comprises:
First by the air dry oven of polybutylene terephthalate PBT at 110 ~ 120 DEG C dry 4 ~ 6 hours, and by the air dry oven of acrylonitrile-butadiene-styrene copolymer ABS at 60 ~ 70 DEG C dry 2 ~ 4 hours;
Take corresponding starting material according to the mass percent of setting again, and taken starting material are joined in high-speed mixer mix; Wherein, described raw-material each constituent mass per-cent is: the PBT of 30 ~ 50%, the ABS of 20 ~ 35%, the compound compatilizer of 1 ~ 5%, the composite toughing agent of 1 ~ 5%, the composite flame-retardant agent of 10 ~ 30%, the compounded lubricant of 0.5 ~ 2%, the composite antioxidant of 0.3 ~ 0.6%, the silicone oil of 0.1 ~ 1%, the tetrafluoroethylene of 0.1 ~ 1% and the Ethyltriphenylphosphonium brimide of 0.1 ~ 0.5%;
Mixture is joined in twin screw extruder again and carry out melting mixing, tank cooling and dicing machine pelletizing operation, obtain described flame retardant plastics matrix material.
As seen from the above technical solution provided by the invention, by the matrix material prepared by the method, there is higher impelling strength and good process industrial art performance, there is excellent flame retardant properties simultaneously, can use in the fields such as automobile, household electrical appliances, electronic information.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme of the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
Fig. 1 provides by the embodiment of the present invention preparation method's schematic flow sheet of flame retardant plastics matrix material;
The structural representation of the twin screw extruder that Fig. 2 provides for the embodiment of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on embodiments of the invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to protection scope of the present invention.
Method described in the embodiment of the present invention uses phosphonium flame retardant; and combine with the novel elastomer-polyphosphonitrile containing a large amount of nitrogen element; composite linear phenolic resin is as the flame-retardant additive of PBT/ABS; be equipped with the components such as compound compatilizer, composite toughing agent and compounded lubricant; the flame retardant plastics matrix material of preparation environmental protection; flame retardant properties is improved greatly, there is high mobility and high toughness simultaneously, can be used for household electrical appliances, automobile, electronics, electrically and the field such as information products.Below in conjunction with accompanying drawing, the embodiment of the present invention is described in further detail, be illustrated in figure 1 the embodiment of the present invention preparation method's schematic flow sheet of flame retardant plastics matrix material is provided, described preparation method comprises:
Step 11: first by the air dry oven of polybutylene terephthalate PBT at 110 ~ 120 DEG C dry 4 ~ 6 hours, and by the air dry oven of acrylonitrile-butadiene-styrene copolymer ABS at 60 ~ 70 DEG C dry 2 ~ 4 hours;
In specific implementation, adopt the intrinsic viscosity of PBT to be 0.75 ~ 0.95dl/g.Here intrinsic viscosity is the sign of molecular weight, and PBT molecular weight is too low, and the impelling strength of alloy is low; Otherwise PBT molecular weight is too high, the poor fluidity of alloy.
Adopt ABS to be high impact grade, melting index (MI) is between 1 ~ 5g/10min (200 DEG C, 5kgf), and high-impact ABS and PBT is blended can obtain the high engineering plastic alloy of impelling strength.
Step 12: take corresponding starting material according to the mass percent of setting again, and taken starting material are joined in high-speed mixer mix;
In this step, specifically can high-speed mixing 1 minute.Above-mentioned raw-material each constituent mass per-cent is: the PBT of 30 ~ 50%, the ABS of 20 ~ 35%, the compound compatilizer of 1 ~ 5%, the composite toughing agent of 1 ~ 5%, the composite flame-retardant agent of 10 ~ 30%, the compounded lubricant of 0.5 ~ 2%, the composite antioxidant of 0.3 ~ 0.6%, the silicone oil of 0.1 ~ 1%, the tetrafluoroethylene of 0.1 ~ 1% and the Ethyltriphenylphosphonium brimide of 0.1 ~ 0.5%;
In specific implementation, the compound compatilizer adopted is that styrene-maleic anhydride copolymer SMA, ethylene butyl acrylate copolymer p TW and styrene-acrylonitrile-glycidyl methacrylate terpolymer SAG is according to the mixed mixture of the mass ratio of 1:1:1.Here, PTW is from also having shock resistance in 40 degrees below zero, and material is pliable and tough, can be used as toughner; EBA polarity is high simultaneously, and various polymer compatibility is good, also has promoter action to the interfacial adhesion improving fire retardant and ABS, PBT simultaneously.Epoxide group on SAG can react with the end carboxyl of PBT, thus plays compatibilization.Three is composite has synergistic effect.
The composite toughing agent adopted is high glue powder, has the MBS MBS of nucleocapsid structure and ethylene vinyl acetate copolymer EVA according to the mixed mixture of the mass ratio of 1:1:1; Wherein, the butadiene content in described high glue powder is 40 ~ 60wt%, and the VA content in described EVA is 22 ~ 30wt%.Here, high glue powder can think the ABS powder that rubber content is high, good with ABS consistency, and toughening effect is given prominence to.MBS has nucleocapsid structure, and shell is Polymers, good with PBT, ABS consistency, and core is the butadiene-styrene copolymer that rubber content is higher, and toughening effect is excellent.The existing good toughening effect of EVA, also can carry heavy alloyed processing fluidity.Three is composite has synergistic effect.
The composite flame-retardant agent adopted is that ethyl hypo-aluminum orthophosphate, zinc borate, linear phenolic resin (softening temperature 75 ~ 90 DEG C) and polyphenylene oxide phosphonitrile (number-average molecular weight is more than 40000) are according to the mixed mixture of the mass ratio of 2:1:1:0.5.Here, ethyl hypo-aluminum orthophosphate is novel halogen-free phosphorus-containing fire retardant agent, particularly has excellent flame retardant effect to polyester (PBT etc.); Zinc borate also has smoke suppressing effect; Linear phenolic resin can improve charring rate, thus has flame retardant effect; Owing to the addition of a large amount of fire retardants, the impact toughness decreased of matrix material, polyphosphonitrile elastomerics not only alloy has excellent flame retardant resistance, and also have excellent toughening effect, toughening effect is good.Therefore, composite flame-retardant agent is phosphorus-nitrogen compound, and charring rate is high simultaneously, smoke-suppressing good, has synergistic effect.
The compounded lubricant adopted is that ethylene bis stearamide EBS, carnauba wax and oxidized polyethlene wax are according to the mixed mixture of the mass ratio of 1:1:1.Here, EBS and carnauba wax can increase mobility and surface quality, and oxidized polyethlene wax also has the dissemination promoting fire retardant, and three is composite has synergistic effect.
The composite antioxidant adopted is that oxidation inhibitor pentaerythritol tetrathioglycollate (i.e. four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester) and GW-540 (i.e. three [2.4-di-tert-butyl-phenyl] phosphorous acid ester) are according to the mixed mixture of the mass ratio of 1:2.
The silicone oil adopted is dimethyl silicone oil, viscosity at 1000 ~ 5000mPa.s, preferably 1500 ~ 3000mPa.s.Here, owing to the addition of a large amount of fire retardants, the mobility of matrix material can receive impact, and therefore add the process flowability that silicone oil improves matrix material, silicone oil has certain flame retardant effect to ABS simultaneously.
The tetrafluoroethylene adopted is Powdered, and median size is 3 ~ 8 μm.Here add tetrafluoroethylene and can suppress drippage, thus reach the fire-retardant rank of UL-94V0.
And adopt Ethyltriphenylphosphonium brimide can carboxyl reaction on catalysis epoxide group and PBT, thus the compatibilization effect of strengthening SAG.
Step 13: mixture is joined in twin screw extruder again and carry out melting mixing, tank cooling and dicing machine pelletizing operation, obtain described flame retardant plastics matrix material.
In this step, described twin screw extruder is the parallel co-rotating twin screw extruder of engagement type;
Be illustrated in figure 2 the structural representation of the twin screw extruder that the embodiment of the present invention provides, in Fig. 2: screw slenderness ratio is 36 ~ 44, screw combinations is moderate shear rate combinations mode, and the temperature of double-screw extruding pelletizing is between 180 ~ 250 DEG C.Here twin screw prilling temperature should not be too high, and shearing force during mixing granulation can not be too strong, otherwise easily cause decomposition and the incipient scorch of ABS, will cause matrix material jaundice like this, mechanical property is inferior and do not have 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 shock strength, the over-all properties of matrix material improves greatly, the dimensional stability of obtained goods increases, there is excellent flame retardant properties, can use in the fields such as automobile, household electrical appliances, electronic information.
For ease of understanding, below in conjunction with concrete enforcement, implementation process of the present invention is described further, under be classified as processing condition prepared by sample in this enforcement:
Adopt SZ-900/NB injector injection molding standard test specimen, molding technological condition: injection temperature (charging opening) 220/230/235/230 DEG C (nozzle), injection pressure 30 ~ 50MPa, dwell time 8s, cooling 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 provides, first by PBT in 110 ~ 120 DEG C of air dry ovens dry 4 ~ 6 hours, by ABS in 60 ~ 70 DEG C of air dry ovens dry 2 ~ 4 hours; Then to weigh each component by formula rate, join in high-speed mixer, high-speed mixing 1 minute; Then mixture is joined melting mixing in twin screw extruder, tank cools, and dicing machine pelletizing, obtains described flame retardant plastics matrix material.
The screw extrusion press used for the parallel co-rotating twin screw extruder of engagement type, screw slenderness ratio be 36 ~ 44, screw combinations is moderate shear rate combinations mode; The temperature (processing condition are shown in Table 2) between 180 ~ 250 DEG C of double-screw extruding pelletizing.
The granulation process parameters of 1-3 implemented by table 2
And then obtained matrix material is detected according to following performance test methods:
Tensile strength and elongation at break: carry out according to GB/T 1040-2006 standard.
Flexural strength and modulus in flexure: carry out according to GB/T 9341-2008 standard.
Notch shock performance: carry out according to GB/T1043-2008 standard.
Heat-drawn wire: carry out according to GB/T1634-2004 standard; Maximum deflection normal stress 1.82MPa, heat-up rate: 2 DEG C/min.
Flame retardant resistance: vertical combustion performance, tests by UL-94 vertical combustion standard, the thick and thick batten of 1.6mm of 3.2mm.
Oxygen index is tested: undertaken by GB/T2406-2008 standard.
Molding shrinkage: undertaken by GB/T 15585-1995 standard.
Implement the performance of the matrix material that 1-3 obtains in table 3:
The performance of table 3 matrix material
As can be seen from the above Table 3, by compound compatilizer, composite toughing agent, composite flame-retardant agent and compounded lubricant modified, prepared matrix material has high melt flow rate (MFR) and high shock strength, the over-all properties of matrix material improves greatly, the dimensional stability of obtained goods increases, compound compatilizer is described, composite toughing agent and compounded lubricant play a good role, may be used for shaping large-scale product, as electric appliance casing, trolley part etc., overcome the shortcoming that flame-retardant PBT/ABS alloy material mobility is bad in the past, reach halogen-free environment-friendly flame-proof simultaneously, to protection of the environment, there is positive contribution.
The above; be only the present invention's preferably embodiment, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.

Claims (10)

1. a preparation method for flame retardant plastics matrix material, is characterized in that, described method comprises:
First by the air dry oven of polybutylene terephthalate PBT at 110 ~ 120 DEG C dry 4 ~ 6 hours, and by the air dry oven of acrylonitrile-butadiene-styrene copolymer ABS at 60 ~ 70 DEG C dry 2 ~ 4 hours;
Take corresponding starting material according to the mass percent of setting again, and taken starting material are joined in high-speed mixer mix; Wherein, described raw-material each constituent mass per-cent is: the PBT of 30 ~ 50%, the ABS of 20 ~ 35%, the compound compatilizer of 1 ~ 5%, the composite toughing agent of 1 ~ 5%, the composite flame-retardant agent of 10 ~ 30%, the compounded lubricant of 0.5 ~ 2%, the composite antioxidant of 0.3 ~ 0.6%, the silicone oil of 0.1 ~ 1%, the tetrafluoroethylene of 0.1 ~ 1% and the Ethyltriphenylphosphonium brimide of 0.1 ~ 0.5%;
Mixture is joined in twin screw extruder again and carry out melting mixing, tank cooling and dicing machine pelletizing operation, obtain described flame retardant plastics matrix material.
2. the preparation method of flame retardant plastics matrix material according to claim 1, is characterized in that,
Adopt the intrinsic viscosity of PBT to be 0.75 ~ 0.95dl/g; Adopt the melting index MI of ABS between 1 ~ 5g/10min.
3. the preparation method of flame retardant plastics matrix material according to claim 1, is characterized in that,
The compound compatilizer adopted is that styrene-maleic anhydride copolymer SMA, ethylene butyl acrylate copolymer p TW and styrene-acrylonitrile-glycidyl methacrylate terpolymer SAG is according to the mixed mixture of the mass ratio of 1:1:1.
4. the preparation method of flame retardant plastics matrix material according to claim 1, is characterized in that,
The composite toughing agent adopted is high glue powder, has the MBS MBS of nucleocapsid structure and ethylene vinyl acetate copolymer EVA according to the mixed mixture of the mass ratio of 1:1:1;
Wherein, the butadiene content in described high glue powder is 40 ~ 60wt%, and the VA content in described EVA is 22 ~ 30wt%.
5. the preparation method of flame retardant plastics matrix material according to claim 1, is characterized in that,
The composite flame-retardant agent adopted is that ethyl hypo-aluminum orthophosphate, zinc borate, linear phenolic resin and polyphenylene oxide phosphonitrile are according to the mixed mixture of the mass ratio of 2:1:1:0.5.
6. the preparation method of flame retardant plastics matrix material according to claim 1, is characterized in that,
The compounded lubricant adopted is that ethylene bis stearamide EBS, carnauba wax and oxidized polyethlene wax are according to the mixed mixture of the mass ratio of 1:1:1.
7. the preparation method of flame retardant plastics matrix material according to claim 1, is characterized in that,
The composite antioxidant adopted is that oxidation inhibitor pentaerythritol tetrathioglycollate and GW-540 are according to the mixed mixture of the mass ratio of 1:2.
8. the preparation method of flame retardant plastics matrix material according to claim 1, is characterized in that,
The silicone oil adopted is dimethyl silicone oil, viscosity at 1000 ~ 5000mPa.s, preferably 1500 ~ 3000mPa.s.
9. the preparation method of flame retardant plastics matrix material according to claim 1, is characterized in that,
The tetrafluoroethylene adopted is Powdered, and median size is 3 ~ 8 μm.
10. the preparation method of flame retardant plastics matrix material according to claim 1, is characterized in that,
Described twin screw extruder is the parallel co-rotating twin screw extruder of engagement type;
Wherein, screw slenderness ratio is 36 ~ 44, and screw combinations is the array mode of moderate shear speed, and the temperature of double-screw extruding pelletizing is between 180 ~ 250 DEG C.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN112724501A (en) * 2020-12-28 2021-04-30 会通新材料股份有限公司 Toughened composite, PBT composite material and preparation method thereof
WO2021227201A1 (en) * 2020-05-13 2021-11-18 佳易容聚合物(上海)有限公司 Use of multi-element random copolymer in improving phase state structure and phase state stability of polyester/styrenic resin alloy

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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.
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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.
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

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
WO2021227201A1 (en) * 2020-05-13 2021-11-18 佳易容聚合物(上海)有限公司 Use of multi-element random copolymer in improving phase state structure and phase state stability of polyester/styrenic resin alloy
CN112724501A (en) * 2020-12-28 2021-04-30 会通新材料股份有限公司 Toughened composite, PBT composite material and preparation method thereof
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

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