CN103360739B - A kind of phosphorus system synergistic fire retardation PC/ABS alloy material and preparation method thereof - Google Patents

A kind of phosphorus system synergistic fire retardation PC/ABS alloy material and preparation method thereof Download PDF

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CN103360739B
CN103360739B CN201310283032.2A CN201310283032A CN103360739B CN 103360739 B CN103360739 B CN 103360739B CN 201310283032 A CN201310283032 A CN 201310283032A CN 103360739 B CN103360739 B CN 103360739B
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abs alloy
flame retardant
abs
alloy material
phosphorus
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CN103360739A (en
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吴宁晶
郎书国
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Heilongjiang Xinda Enterprise Group Co Ltd
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Qingdao University of Science and Technology
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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
    • B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
    • B29C48/911—Cooling
    • 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
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • 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
    • 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
    • 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
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895—Barrel or housing

Abstract

Disclosure one phosphorus system synergistic fire retardation PC/ABS alloy material, it is characterised in that PC/ABS alloy resin 50.0-94.0wt%, phosphorus flame retardant 5.0-40.0wt%, nitrogenated flame retardant 0.0-30.0wt%, silicon system synergist 0.0-10.0wt%, bulking agent 0.5-20.0wt, antioxidant 0.5-1.0wt%；Wherein in PC/ABS alloy material, PC content is 90.0-10.0wt%, ABS content is 10.0-90.0wt%, and above component is all weight percentage。A kind of phosphorus system provided by the invention synergistic fire retardation PC/ABS alloy material, adopts phosphorus flame retardant and nitrogenated flame retardant compound or phosphorus flame retardant and the collaborative use of silicon system synergist, the preparation method adopting melt blending extrusion。The physical properties such as the mechanics of halogen-free flame retardant PC/ABS alloy material, processing, thermostability and electrical property can be promoted on the one hand；Can improving the flame retarding efficiency of fire retardation PC/ABS alloy material on the other hand, reduce in combustion process and discharge toxic gas volume, the few poison of low cigarette, is a kind of environmentally friendly fire proofing。

Description

A kind of phosphorus system synergistic fire retardation PC/ABS alloy material and preparation method thereof
Technical field
The invention belongs to halogen-free flame retardant PC/ABS alloy material, be specifically related to a kind of phosphorus system synergistic fire retardation PC/ABS alloy material and preparation method thereof。
Background technology
Merlon (PC) is strand constitutional repeating unit is the polymer of carbonate。The advantages such as PC has impact strength height, creep resistance and good stability of the dimension, heat-resisting, transparent, water absorption rate is low, nontoxic, dielectric properties are excellent, at electric, auto industry, medical apparatus and instruments, building and lighting apparatus and many high-technology fields, such as the field such as Aeronautics and Astronautics, electronic computer, optical fiber is of many uses；But, PC there is also processing fluidity stress cracking poor, easy, to shortcomings such as notch sensitive, easily abrasion, chemical proofing are poor, on the high side, and these shortcomings make its application in a lot of fields be restricted。
ABS is acrylonitrile-butadiene-styrene copolymer or the blend of acrylonitrile/cinnamic copolymer and styrene/butadiene copolymers, English name is Acrylonitrile-Butadiene-Styrene (ABS), it is the graft copolymer mixture with acrylonitritrile-styrene resin of butadiene, wherein acrylonitrile accounts for 15%-35%, butadiene accounts for 5%-30%, and styrene accounts for 40-60%。Along with the change of three kinds of component ratios, the performance that the physical and mechanical properties of PC/ABS resin changes therewith is between general-purpose plastics and engineering plastics, and its shock resistance is good, mobility is excellent, but its thermostability and weatherability are poor, and mechanical property is not ideal enough, therefore cause that its application is limited。
The shortcoming that the alloy of PC/ABS can overcome two kinds of raw materials self, the advantage developing the other side, after both generals are blended, one can improve the thermostability of PC/ABS, impact and hot strength, it two can reduce polycarbonate melt viscosity, improves processing characteristics, reduces PC notch sensitivity, improve PC stress cracking situation, reduce production cost。Making PC/ABS alloy be developed rapidly and apply especially because PC/ABS alloy provides better overall cost and excellent low temperature notched impact strength, its development speed has exceeded the development speed of other alloy of ABS and PC。Overall superior thermostability, intensity and processability are the reasons that PC/ABS alloy is developed rapidly, and therefore PC/ABS alloy has more wide application market
PC/ABS alloy material is used widely in the automotive industry, as being used for making the parts such as instrument board, bumper, vehicle-body outer panel, internal and external ornament part, it is also possible in office machine such as photocopier, typewriter and computer etc.。In recent years, in order to meet at electronics, the particular/special requirement of the application fire safeties such as electric product, PC/ABS alloy must with excellent fire resistance, and the flame-retarded technology of PC/ABS alloy becomes the focus of people's research。Along with the cry of environmental protection and safety is grown to even greater heights by people, material environment friendly is required more and more higher。And the halogenated flame retardants such as decabromodiphenyl oxide conventional at present can produce toxic, corrosive gas and a large amount of smog when material thermal cracking and burning and contaminated environment, secondary public hazards, the promulgation of two instructions of ROHS and WEEE that European Union puts into effect for 2003 are caused to limit tradition halogen system fire retardation PC/ABS application in a lot of industries especially。Thus under the situation that the non-halogen cry of fire proofing is day by day surging, domestic and international researcher starts to be applied to all kinds of halogen-free flame retardants PC/ABS alloy, to obtaining the halogen-free flame retardant PC/ABS product of few cigarette, low toxicity, high-efficiency environment friendly green。
At present, the halogen-free flame-retardant system of PC/ABS alloy includes phosphorous system, nitrogen system, silicon-series five-retardant, inorganic fire-retarded system and Intumescent Retardant System。Aluminium hydroxide and magnesium hydroxide are two kinds of the most commonly used inorganic combustion inhibitors, have nontoxic, press down cigarette, the advantage such as cheap, but the flame retarding efficiency of inorganic powdered filler is relatively low, addition reaches more than 40% and its is possible to reach UL94V-0 flame retardant rating, additionally inorganic combustion inhibitor and PC/ABS alloy poor compatibility, high amount of inorganic filler makes the mechanical properties decrease of material in PC/ABS alloy resin serious, and outward appearance and processing characteristics and electrical property sharply worsen。Intumescent Retardant System mainly includes acid source, charcoal source and source of the gas three elements, wherein with APP, tetramethylolmethane and tripolycyanamide for representative, have nontoxic, press down the advantages such as cigarette, but there is exudative and water miscible problem in tetramethylolmethane, and Intumescent Retardant System is incompatible with polymer, mechanical property and the resistance to water of polymer also can be reduced, so Intumescent Retardant System is also restrained in the application of PC/ABS after addition。
In traditional phosphorous flame-retardant system, triphenyl (Triphenylphosphate, TPP) and when derivant is applied in PC/ABS alloy, owing to the volatilization temperature of TPP is lower than the processing temperature of PC/ABS alloy, cause that TPP is volatile in the PC/ABS alloy course of processing to ooze out。The t-butyl phosphate triphenylmethyl methacrylate improved on TPP basis is more more superior than TPP fire resistance, and it is a kind of liquid combustion inhibitor, and in resin, persistency and hydrolytic stability are more preferably, and is not likely to produce surface stress be full of cracks, but it still has higher volatility。Tetramethylolmethane spiro-phosphate (PSDPP) flame retarding efficiency in PC/ABS alloy is high, and the TPP of the PSDPP and mass fraction 3.5% that only add mass fraction 3.8% is just enough to make PC/ABS alloy reach V-0 level。But tetramethylolmethane spiro-phosphate fire retardant has higher volatility and water solublity so that it is be difficult to be applied in PC/ABS alloy。
For above-mentioned reason, select heat stability higher and the phosphorus flame retardant of water-tolerant and introduce synergist in phosphorus flame retardant and can be effectively improved the flame retarding efficiency of PC/ABS alloy。Therefore, the present invention adopts phosphorus flame retardant fire retardation PC/ABS alloy material, and adding nitrogenated flame retardant or silicon system synergist, that PC/ABS alloy carries out synergistic is fire-retardant, to reduce the consumption of fire retardant, improves the flame retarding efficiency of phosphorous flame-retardant PC/ABS alloy material。
Summary of the invention
It is an object of the invention to for halogen-free flame retardants, the flame retarding efficiency of PC/ABS alloy is low and heat stability and poor water resistance shortcoming, a kind of phosphorus system synergistic halogen-free flame retardant PC/ABS alloy material is provided, the fire retardation PC provided in the present invention/ABS alloy material adopts phosphorus system and nitrogenated flame retardant or phosphorus flame retardant and the collaborative use of silicon system synergist, the flame retarding efficiency of halogen-free flame retardant PC/ABS alloy material can be improved on the one hand, promote the comprehensive mechanical property of halogen-free flame retardant PC/ABS alloy material, thermostability, electrical property etc.；And reduce the poisonous gas discharged in combustion process, the few poison of low cigarette。Therefore the phosphorus system synergistic fire retardation PC/ABS alloy material in the present invention is a kind of environmentally friendly fire proofing。
1. a kind of phosphorus system provided by the invention synergistic fire retardation PC/ABS alloy material, it is characterised in that this material is made up of following component:
PC/ABS alloy 50.0-94.0wt%
Phosphorus flame retardant 5.0-40.0wt%
Nitrogenated flame retardant 0.0-30.0wt%
Silicon system synergist 0.0-10.0wt%
Bulking agent 0.5-20.0wt%
Antioxidant 0.5-1.0wt%
Above component is all weight percentage, wherein the preferred 60.0-90.0wt% of PC/ABS alloy, the preferred 8.0-25.0wt% of phosphorus flame retardant, the preferred 0.0-20.0wt% of nitrogenated flame retardant, the preferred 0.0-4.0wt% of silicon system synergist, the preferred 2.0-15.0wt% of bulking agent, the preferred 0.5-0.8wt% of antioxidant。
2. in PC/ABS alloy resin contained in above-mentioned phosphorus system synergistic fire retardation PC/ABS alloy material, weight percent content 90.0-10.0wt%, the ABS weight percent content 10.0-90.0wt% of contained PC。
3. phosphorus flame retardant contained in above-mentioned phosphorus system synergistic fire retardation PC/ABS alloy material includes the one in phosphate, Quadrafos, pyrophosphate, inorganic hypophosphites, organic hypophosphites。
4. nitrogenated flame retardant contained in above-mentioned phosphorus system synergistic fire retardation PC/ABS alloy material includes the one in tripolycyanamide, cyanurate melamine salt, dicyandiamide, melamine and salt thereof and guanidinesalt。
5. silicon system synergist contained in above-mentioned phosphorus system synergistic fire retardation PC/ABS alloy material includes the one in silane, dimethyl siloxane, methyl phenyl siloxane, silicones, polysilsesquioxane (POSS)。
6. bulking agent contained in above-mentioned phosphorus system synergistic fire retardation PC/ABS alloy material includes maleic anhydride grafted polystyrene, glycidyl methacrylate graft polystyrene, maleic anhydride grafted ABS, glycidyl methacrylate graft ABS, glycidyl methacrylate graft styrene-butadiene-styrene block copolymer (SBS), Maleic anhydride-containg polyethylene, maleic anhydride graft rubber, glycidyl methacrylate graft rubber, vinyl-acrylate copolymer, methacrylate copolymer, one in ethylene-acrylate-glycidyl methacrylate copolymer
7. the preparation method of a kind of phosphorus system provided by the invention synergistic fire retardation PC/ABS alloy material is the method adopting melt blending extrusion, and concrete technical process and blending condition are as follows:
(1) using dried fire retardant, synergist, bulking agent and antioxidant by proportioning in high-speed mixer mix homogeneously as the built agent of fire retardant。
(2) by the built agent of PC/ABS alloy and fire retardant, joining melt blending extrusion in double screw extruder, the temperature that double screw extruder is each section is 180-280 DEG C, melt extrudes rear cooling granulation。
Detailed description of the invention
By the following examples the present invention is specifically described; it is important to point out that following example are served only for that the invention will be further described; it is not intended that limiting the scope of the invention; some nonessential improvement and adjustment that the present invention is made by the person skilled in the art in this field according to the invention described above content, still fall within scope。
Embodiment 1
By 10.0wt% APP, 2.0wt% cyanurate melamine salt, 2.0wt%SBS grafted maleic anhydride, 0.5wt% antioxidant (0.25wt%1010 and 0.25wt%168) puts into and prepares composite flame-proof modifier in high-speed mixer after mix homogeneously, then with 85.5wt%PC/ABS alloy resin (weight ratio 70:30), it is respectively put in double screw extruder, melt extrudes in 200-250 DEG C, and cooling granulation。The LOI of the phosphorus system cooperative flame retardant PC/ABS alloy material of gained is 26.5%, and UL94 vertical combustion rank is V-0。
Embodiment 2
By 10.0wt% aminomethyl phenyl hypo-aluminum orthophosphate, 2.0wt% dimethyl siloxane, 6.0wt%SBS grafted methacrylic acid glyceride, 0.5wt% antioxidant (0.25wt%1010 and 0.25wt%168) puts into and prepares composite flame-proof modifier in high-speed mixer after mix homogeneously, then with 81.5wt%PC/ABS alloy (weight ratio 70:30), enter in double screw extruder respectively through charge door, melt extrude at 200-250 DEG C, and cooling granulation。The LOI of the phosphorus system cooperative flame retardant PC/ABS alloy material of gained is 27.0%, and vertical combustion grade is UL94V-0。
Embodiment 3
By 15.0wt% diethyl hypo-aluminum orthophosphate, 2.0wt% cyanurate melamine salt, 6.0wt%SBS grafted methacrylic acid glyceride, 0.5% antioxidant (0.25wt%1010 and 0.25wt%168) is put into and is prepared composite flame-proof modifier in high-speed mixer after mix homogeneously, then with the PC/ABS alloy resin (weight ratio 50:50) of 81.5.0wt%, enter in double screw extruder respectively through charge door, 190-240 DEG C melt extrudes, and cooling granulation。The LOI of the PC/ABS alloy material of the phosphorus system cooperative flame retardant of gained is 27.0, UL94 vertical combustion ranks is V-0。
Embodiment 4
By 18.0wt% hypo-aluminum orthophosphate, 2.0wt% silicones, 6.0wt% polystyrene graft maleic anhydride, 0.5% antioxidant (0.25wt%1010 and 0.25wt%168) is put into and is prepared composite flame-proof modifier in high-speed mixer after mix homogeneously, then with the PC/ABS alloy resin (weight ratio 50:50) of 73.5wt%, enter in double screw extruder respectively through charge door, melt extrude in 190-240 DEG C, and cooling granulation。The LOI of the halogen-free flame retardant PC/ABS alloy material of gained is 26.5, UL94 vertical combustion ranks is V-0。
Embodiment 5
By 20.0wt% diethyl hypo-aluminum orthophosphate, 2.0wt% polysilsesquioxane (POSS), 6.0wt%ABS grafted methacrylic acid glyceride, 0.5wt% antioxidant is put into and is prepared composite flame-proof modifier in high-speed mixer after mix homogeneously, then mix homogeneously with 71.5wt%PC/AB alloy resin (weight ratio 30:70), add in double screw extruder, 180-230 DEG C melt extrudes, and cooling granulation。The LOI of the PC/ABS alloy material of the halogen-free flameproof of gained is 26.0, UL94 vertical combustion ranks is V-0。
Embodiment 6
By 22.0wt% APP, 6.0wt% cyanurate melamine salt, 4.0wt%SBS alloy grafted methacrylic acid glyceride, 0.5wt% antioxidant (0.25wt%1010 and 0.25wt%168) puts into and prepares composite flame-proof modifier in high-speed mixer after mix homogeneously, then with 67.5wt%PC/ABS alloy resin (weight ratio 30:70), enter in double screw extruder respectively through charge door, 180-230 DEG C melt extrudes, and cooling granulation。The LOI of the phosphorus system cooperative flame retardant PC/ABS alloy material of gained is 25.0%, and UL94 vertical combustion rank is V-1。

Claims (3)

1. phosphorus system synergistic fire retardation PC/ABS alloy material, it is characterised in that this material is made up of following component:
PC/ABS alloy resin 60.0-90.0wt%, the composition of described PC/ABS alloy resin includes PC content 70.0-30.0wt%, ABS content 30.0-70.0wt%；The consumption of phosphorus flame retardant is 0.39 times of ABS content, 0.40 times, 0.41 times, 0.47 times or 0.49 times, bulking agent 2.0-15.0wt%, antioxidant 0.5-0.8wt%, additionally possibly together with synergistic flame retardant, described synergistic flame retardant is the one in nitrogenated flame retardant 2-6wt% or silicon system synergist 2wt%；
Above constituent content sum is 100%；
Contained phosphorus flame retardant includes phosphate, Quadrafos, any one in pyrophosphate, inorganic hypophosphites, organic hypophosphites；
Contained nitrogenated flame retardant includes any one in tripolycyanamide, MCA, dicyandiamide, melamine and guanidinesalt thereof；
Contained silicon system synergist is any one in silane, dimethyl siloxane, methyl phenyl siloxane, silicones, polysilsesquioxane。
2. phosphorus system according to claim 1 synergistic fire retardation PC/ABS alloy material, it is characterized in that contained bulking agent is maleic anhydride grafted polystyrene, glycidyl methacrylate graft polystyrene, maleic anhydride grafted ABS, glycidyl methacrylate graft ABS, glycidyl methacrylate graft SBS, Maleic anhydride-containg polyethylene, maleic anhydride graft rubber, glycidyl methacrylate graft rubber, vinyl-acrylate copolymer, methacrylate copolymer, any one in ethylene-acrylate-glycidyl methacrylate copolymer。
3. the preparation method of phosphorus system according to claim 1 synergistic fire retardation PC/ABS alloy material is the method adopting melt blending extrusion, concrete technical process:
(1) using dried fire retardant, synergistic flame retardant, bulking agent, antioxidant by proportioning in high-speed mixer mix homogeneously as the built agent of fire retardant；
(2) after the built agent mix homogeneously of PC/ABS alloy resin and fire retardant, joining melt blending extrusion in double screw extruder, the temperature range that double screw extruder is each section is 180-280 DEG C, melt extrudes rear cooling granulation。
CN201310283032.2A 2013-07-08 2013-07-08 A kind of phosphorus system synergistic fire retardation PC/ABS alloy material and preparation method thereof Expired - Fee Related CN103360739B (en)

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CN103756243A (en) * 2014-01-02 2014-04-30 广东聚石化学股份有限公司 Cold-resisting halogen-free inflaming retarding ABS (Acrylonitrile Butadiene Styrene) and preparation method thereof
CN104592731B (en) * 2015-01-27 2016-06-15 奉化市兴杨塑业有限公司 A kind of silicon system fire retardation PC/ABS
CN112679935A (en) * 2020-12-25 2021-04-20 青岛中新华美塑料有限公司 Highlight extrusion halogen-free flame-retardant PC/ABS alloy material, preparation method thereof and obtained product
CN113583421B (en) * 2021-08-11 2022-12-13 上海品诚控股集团有限公司 High-transparency low-YI-value halogen-free flame-retardant PC material and preparation method thereof

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CN102061077A (en) * 2010-12-31 2011-05-18 南京金杉汽车工程塑料有限责任公司 Halogen-free inflaming retarding PC/ABS (Polycarbonate/Acrylonitrile Butadiene Styrene) alloy
CN102399412A (en) * 2011-11-09 2012-04-04 金发科技股份有限公司 Halogen free flame resistant ABS composition with low cost and high performance, and preparation method and application thereof

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CN102399412A (en) * 2011-11-09 2012-04-04 金发科技股份有限公司 Halogen free flame resistant ABS composition with low cost and high performance, and preparation method and application thereof

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CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20160622

Termination date: 20210708