CN102775754A - Halogen-free composite flame retardant poly carbonates (PC)/acrylonitrile butadiene styrene copolymers (ABS) alloy and preparation method thereof - Google Patents
Halogen-free composite flame retardant poly carbonates (PC)/acrylonitrile butadiene styrene copolymers (ABS) alloy and preparation method thereof Download PDFInfo
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- CN102775754A CN102775754A CN2012102591543A CN201210259154A CN102775754A CN 102775754 A CN102775754 A CN 102775754A CN 2012102591543 A CN2012102591543 A CN 2012102591543A CN 201210259154 A CN201210259154 A CN 201210259154A CN 102775754 A CN102775754 A CN 102775754A
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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
- 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
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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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- 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
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Abstract
The invention discloses a halogen-free composite flame retardant PC/ABS alloy and a preparation method thereof. The alloy is composed by, by weight, 50-90 parts of poly carbonates containing flame retardant master batch, 8-40 parts of ABS, 2-8 parts of polyborosiloxane and 0.1-1.5 parts of teflon, wherein the flame retardant master batch is produced by 95-99 parts of PC by weight and 1-5 parts sulphosalts flame retardant of by weight. The alloy is excellent in flame retardance, good in mechanical property, environmental-friendly, and suitable for application fields such as electronics, electrical appliances and automobiles.
Description
Technical field
The invention belongs to high molecule alloy material and preparing technical field thereof, relate in particular to a kind of Halogen composite flame-proof PC/ABS Alloy And Preparation Method.
Background technology
Polycarbonate/acrylonitrile-butadiene-phenylethene copolymer alloy (PC/ABS alloy) is a kind of important engineering polyblend, and this alloy has the two premium properties of polycarbonate (PC) and acrylonitrile-butadiene-styrene copolymer (ABS) simultaneously.The thermotolerance of blend alloy, shock strength and tensile strength are superior to ABS; Its melt viscosity is lower than PC simultaneously, and processing characteristics is better than PC, and goods internal stress and shock strength all reduce the susceptibility of products thickness greatly, and dimensional stability is good, is particularly suitable for the manufacturing of thin-gage goods.Therefore the PC/ABS alloy is widely used in a plurality of fields such as automobile, electrical equipment, office equipment, Communication Equipments in recent years.
Yet the PC/ABS alloy material is owing to the limitation of self structure, and its flame retardant properties is relatively poor.PC itself has certain self-extinguishing, and flame retardant properties is preferably arranged, but ABS is a kind of inflammable macromolecular material; Its oxygen index lower (being about 17%); Combustionvelocity is very fast, and the PC/ABS alloy flame retardant properties that PC and ABS blend make obviously reduces, and can not satisfy the application requiring in many fields; Make its application receive very big restriction, so fire retardation PC/ABS alloy exploitation has become a focus of current fire-retardant research field.
The PC/ABS alloy adopts halogenated flame retardant mostly for a long time, bromide fire retardant especially, advantage such as this based flame retardant has the flame retarding efficiency height, and consumption is low.But, the harm that requires increasingly high, traditional halogenated flame retardant to bring of material environment friendly is highlighted day by day along with the progress of science and technology.Therefore, research and development efficient and environment-friendly type halogen-free flame retardant PC/ABS alloy just becomes the important topic of environment protection.The halogen-free flameproof of PC/ABS alloy mainly adopts inorganic phosphorus system, organophosphorus system (mainly being phosphoric acid ester), silicone based flame retardant etc.Like publication number is that the one Chinese patent application of CN101173090 discloses a kind of halogen-free flame retardant PC/ABS alloy; Adopt 10 ~ 18 parts of phosphoric acid ester fire retardants (triphenylphosphate, triphenyl phosphite etc.), Marinco H 1 ~ 2 cooperative flame retardant PC/ABS alloy; Make alloy material reach UL94 (1.6mm) V-0 level, the phosphoric acid ester fire retardant also makes the processing fluidity of PC/ABS alloy improve simultaneously.And for example publication number is that the Chinese patent of CN101173089 adopts the composite flame-retardant agent be made up of phosphoric acid ester fire retardant, sulphonate and siloxanes that the PC/ABS alloy is carried out fire-retardant finish, obtains flame retardant effect preferably.In the fire-retardant finish of PC/ABS alloy; Though the addition of fire retardant can make the PC/ABS alloy obtain comparatively ideal flame retardant effect greatly; But tend to bring negative impact, therefore, make by fire retardant material and obtain the ideal flame retardant effect to the mechanical property of alloy material; Keep material good mechanical performance simultaneously, the research and development efficient flame-retarding agent is most important.Yet the fire retardant addition is low excessively, as is lower than 0.1%, is difficult in the PC/ABS alloy to be uniformly dispersed, and makes the flame retardant properties of material unstable, and therefore, making fire retardant can homodisperse be the key factor that obtains the high-performance refractory material in plastics substrate.
Summary of the invention
The objective of the invention is deficiency to prior art; Provide that a kind of flame retardant properties is good, the Halogen composite flame-proof PC/ABS Alloy And Preparation Method of good mechanical performance, environmental protection, this halogen-free flame retardant PC/ABS alloy can be widely used in electronic apparatus, the automotive industry.
Halogen composite flame-proof PC/ABS alloy, described alloy is processed by the raw material that comprises following weight part:
50～90 parts of polycarbonate that contain fire-retardant master granule;
8～40 parts of acrylonitrile-butadiene-styrene copolymers (ABS);
2～10 parts of polyborosiloxanes;
0.1～1.5 part of tetrafluoroethylene;
The described polycarbonate that contains fire-retardant master granule is processed by following raw materials by weight percent:
Fire-retardant master granule 10%～20%;
Polycarbonate (PC) surplus.
Described fire-retardant master granule is processed by the raw material that comprises following weight part:
95～99 parts of PC;
1～5 part of Sulfonates fire retardant.
Described Sulfonates fire retardant is perfluoro butyl potassium sulfonate, perfluoro butyl sodium sulfonate or sulfobenzide potassium sulfonate.
Halogen composite flame-proof PC/ABS alloy preparation method specifically comprises as follows:
Sulfonates fire retardant efficient that the present invention selected for use is high, used addition seldom, in fire retardation PC/ABS alloy total amount; Addition is less than 1% (0.05～0.9%); Will sulphonate directly be mixed being difficult to be uniformly dispersed with PC/ABS and other component, fire retardant can not will cause the flame retardant properties of alloy material unstable by homodisperse in matrix, and some part flame retardant properties of material is good; And some part flame retardant properties is relatively poor; Can not satisfy request for utilization, the present invention adopts earlier the Sulfonates fire retardant with higher addition and the compound fire-retardant master granule of processing of PC, and then is undertaken compound by proportioning and PC, ABS and other component fire-retardant master granule; Realize the homodisperse of Sulfonates fire retardant in PC/ABS matrix, improved the overall performance of alloy material; Fire-retardant master granule prepares as follows:
PC and Sulfonates fire retardant by after the proportioning pre-mixing, were mixed 3 minutes～8 minutes down in 250 ℃～270 ℃ in torque rheometer, make fire-retardant master granule, screw speed is 50r/min～100r/min in the described torque rheometer;
Or, make fire-retardant master granule with in twin screw extruder, melt extruding granulation in 255 ℃～280 ℃ after PC and the pre-mixing of Sulfonates fire retardant.
The another kind of fire retardant that the present invention adopts is a polyborosiloxane, and organic side group of described polyborosiloxane comprises C
1～C
4Alkyl, phenyl, tolyl, C
2～C
4Alkene class unsaturated alkyl in one or more, contain methyl and phenyl simultaneously in the side group of preferred polyborosiloxane.
Polyborosiloxane is owing to contain two kinds of ignition-proof elements simultaneously in molecular structure: silicon and boron exist flame retardant synergistic effect, thereby have flame retardant properties more efficiently than general ZGK 5.
The mol ratio of silicon and boron is (0.3～3) in the described polyborosiloxane: 1, be preferably (0.5～2): 1.The fire-retardant synergy of silicon, boron is best in the polyborosiloxane in this proportional range, in addition, is lower than this ratio, and the product resistance to water soak is poor.
Polyborosiloxane weight-average molecular weight≤15000 that described the present invention selects for use; The molecular weight of polyborosiloxane too high then with PC/ABS consistency variation, in alloy, disperse unevenly, influence the flame retardant properties and the mechanical property of material.
The preparation method of described polyborosiloxane may further comprise the steps:
Step (1). in water, add acetate or hydrochloric acid, add silane again, regulate pH value to 1.8～5.0; The mol ratio of silane and water is 1: (3～20); Stir hydrolysis 20 minutes～120 minutes at 60 ℃～90 ℃, generate silanol, add organic solvent then and form reaction soln;
Described silane is two functionality organosilane R
2SiX
2, three-functionality-degree organosilicon alkane RSiX
3Or their mixture, R
2SiX
2Or RSiX
3Organic radical R in the formula is selected from C
1～C
4Alkyl, C
2～C
4Alkene class unsaturated alkyl, phenyl, tolyl in a kind of, X is an alkoxyl group;
Step (2). in above-mentioned reaction soln, add boric acid, 70 ℃～120 ℃ reactions 2 hours～10 hours, underpressure distillation removed and desolvates, and obtains polyborosiloxane.
Organic solvent in the described step (1) is selected from one or more mixtures in hexane, heptane, methylpentane, toluene, the YLENE.
At last; Polycarbonate, fire-retardant master granule, acrylonitrile-butadiene-styrene copolymer, polyborosiloxane, tetrafluoroethylene are carried out pre-mixing in high-speed mixer; Again pre-composition is melt extruded granulation on twin screw extruder; Extruder temperature is at 230～255 ℃, rotating speed 200～240r/min.
Beneficial effect of the present invention is following:
In PC/ABS compound system of the present invention, the Sulfonates fire retardant can quicken the rate of decomposition of PC in combustion processes, promotes the crosslinked of PC and becomes charcoal.The present invention adopts earlier Sulfonates fire retardant and the compound fire-retardant master granule of processing of PC, and then fire-retardant master granule is undertaken compound by proportioning and PC, ABS and other component, makes the sulphonate can homodisperse in matrix, brings into play better fire-retardant effectiveness.Polyborosiloxane can promote the crosslinked of PC/ABS alloy in combustion processes; Generate borosilicate glass class and Si-C crosslinking structure; Form the densification that contains Si and B, uniform charcoal layer at composite material surface; Polyborosiloxane and sulphonate act synergistically in the PC/ABS compound system, in combustion processes, promote to form more more compact carbon layer, and this charcoal layer plays the effect of good insulation resist; The infiltration and the inflammable gas that have effectively hindered oxygen and heat are diffused into the combustion zone, thereby the flame retardant properties of material is effectively improved.In addition, very little when polyborosiloxane plays fire retardation to the PC/ABS alloy to the negative impact of alloy mechanical property, even the also improvement to some extent of performance to having.Fire retardation PC/ABS alloy the flame retardant properties of the present invention's preparation is good, and mechanical property is good, and environmental protection is applicable to Application Areass such as electronics, electrical equipment, automobile.
Embodiment
Following embodiment further specifies of the present invention, rather than limits scope of the present invention.
The employed main raw material of following examples is following:
Polycarbonate (PC): CALIBRE201-10, LG DOW polycarbonate ltd;
ABS:AG15E1, platformization (Ningbo) plastic cement ltd;
Perfluoro butyl potassium sulfonate: FR-2025, Minnesota Mining and Manufacturing Company;
Sulfobenzide potassium sulfonate: KSS-FR, U.S. SLOSS company;
Polytetrafluoroethylene (PTFE): Aladdin chemistry ltd.
PC and ABS will carry out drying, PC:102 ℃/24h in air dry oven before using in following embodiment; ABS:80 ℃/8h.
Embodiment 1
In the there-necked flask of 500ml, add 160g water and small amount of acetic acid; The dimethoxydiphenylsilane of 49g, the phenyltrimethoxysila,e of 32g and the mixture of 30g dimethyldimethoxysil,ne are poured in the constant pressure funnel; Dropwise add in the above-mentioned flask; Adjustment pH value to 1.8 was reacted 120 minutes down at 60 ℃, got the intermediate product silanol.Then the synthetic silanol is dissolved in the 120g YLENE, the xylene solution of silanol is continued 120 ℃ of reactions 2 hours down with 22g boric acid again, solvent xylene is removed in underpressure distillation, finally obtains the polyborosiloxane fire retardant.
Embodiment 2
In the there-necked flask of 500ml, add 140g water and small amount of hydrochloric acid; The dimethoxydiphenylsilane of 60g and the mixture of 36g dimethyldimethoxysil,ne are poured in the constant pressure funnel; Dropwise add in the above-mentioned flask; Adjustment pH value to 5.0 was reacted 20 minutes down at 90 ℃, got the intermediate product silanol.Then the synthetic silanol is dissolved in the 130g toluene, the toluene solution of silanol is continued 70 ℃ of reactions 10 hours down with 19g boric acid again, solvent toluene is removed in underpressure distillation, finally obtains the polyborosiloxane fire retardant.
Embodiment 3
In the there-necked flask of 500ml, add 170g water and small amount of hydrochloric acid; The dimethoxydiphenylsilane of 73g and the mixture of 36g dimethyldimethoxysil,ne are poured in the constant pressure funnel; Dropwise add in the above-mentioned flask; Adjustment pH value to 2.5 was reacted 80 minutes down at 80 ℃, got the intermediate product silanol.Then the synthetic silanol is dissolved in the 130g toluene, the toluene solution of silanol is continued 100 ℃ of reactions 6 hours down with 37g boric acid again, solvent toluene is removed in underpressure distillation, finally obtains the polyborosiloxane fire retardant.
Embodiment 4
After PC99 part (weight part, as follows) and 1 part of pre-mixing of perfluoro butyl potassium sulfonate (FR-2025), in torque rheometer, under the 60rpm rotating speed, mixed 7 minutes down in 265 ℃, make fire-retardant master granule.
5 parts of polyborosiloxane fire retardants and tetrafluoroethylene that 7 parts of above-mentioned fire-retardant master granules, PC58 part, ABS30 part, embodiment 1 are made mix for 0.5 part; Join in the twin screw extruder then; At 255 ℃ of following extruding pelletizations, make fire retardation PC/ABS alloy material PC/ABS-1.
Embodiment 5
After PC96 part (weight part, as follows) and 4 parts of pre-mixings of perfluoro butyl potassium sulfonate (FR-2025), in torque rheometer, under the 50rpm rotating speed, mixed 8 minutes down in 250 ℃, make fire-retardant master granule.
2 parts of polyborosiloxane fire retardants and tetrafluoroethylene that 10 parts of above-mentioned fire-retardant master granules, PC48 part, ABS40 part, embodiment 1 are made mix for 0.3 part; Join in the twin screw extruder then; At 250 ℃ of following extruding pelletizations, make fire retardation PC/ABS alloy material PC/ABS-2.
Embodiment 6
8 parts of (weight parts of fire-retardant master granule that embodiment 5 is made; As follows), PC64 part, ABS20 part, embodiment 18 parts of the polyborosiloxane fire retardants and the tetrafluoroethylene that make mix for 0.8 part; Join in the twin screw extruder then; At 245 ℃ of following extruding pelletizations, make fire retardation PC/ABS alloy material PC/ABS-3.
Embodiment 7
After PC98 part (weight part, as follows) and 2 parts of pre-mixings of sulfobenzide potassium sulfonate (KSS-FR), in torque rheometer, under the 70rpm rotating speed, mixed 5 minutes down in 265 ℃, make fire-retardant master granule.
4 parts of polyborosiloxane fire retardants and tetrafluoroethylene that 9 parts of above-mentioned fire-retardant master granules, PC68 part, ABS19 part, embodiment 2 are made mix for 0.6 part; Join in the twin screw extruder then; At 245 ℃ of following extruding pelletizations, make fire retardation PC/ABS alloy material PC/ABS-4.
Embodiment 8
After PC95 part (weight part, as follows) and 5 parts of pre-mixings of sulfobenzide potassium sulfonate (KSS-FR), in torque rheometer, under the 100rpm rotating speed, mixed 8 minutes down in 255 ℃, make fire-retardant master granule.
10 parts of polyborosiloxane fire retardants and tetrafluoroethylene that 9 parts of above-mentioned fire-retardant master granules, PC73 part, ABS8 part, embodiment 3 are made mix for 0.1 part; Join in the twin screw extruder then; At 235 ℃ of following extruding pelletizations, make fire retardation PC/ABS alloy material PC/ABS-5.
Comparative Examples
The PC of 80 weight parts and the ABS of 20 weight parts are mixed, join then in the twin screw extruder,, make PC/ABS alloy material PC/ABS-0 at 245 ℃ of following extruding pelletizations.
The performance of above-mentioned PC/ABS alloy material sees shown in the table 1 that tensile strength is according to GB/T 1040.2-2006 standard testing; Flexural strength is according to GB/T 9341-2008 standard testing; Notched Izod impact strength is according to GB/T 1043.1-2008 standard testing; Limiting oxygen index determination carries out according to GB/T 2406.2-2009 standard.
[0035] table 1
Claims (8)
1. Halogen composite flame-proof PC/ABS alloy, process by the raw material that comprises following weight part:
50～90 parts of polycarbonate that contain fire-retardant master granule;
8～40 parts of acrylonitrile-butadiene-styrene copolymers;
2～10 parts of polyborosiloxanes;
0.1～1.5 part of tetrafluoroethylene;
The described polycarbonate that contains fire-retardant master granule is processed by following raw materials by weight percent:
Fire-retardant master granule 10%～20%;
The polycarbonate surplus.
2. Halogen composite flame-proof PC/ABS alloy according to claim 1 is characterized in that described fire-retardant master granule is processed by the raw material that comprises following weight part:
95～99 parts of polycarbonate;
1～5 part of Sulfonates fire retardant.
3. Halogen composite flame-proof PC/ABS alloy according to claim 1 is characterized in that organic side group of described polyborosiloxane comprises C
1～C
4Alkyl, phenyl, tolyl, C
2～C
4Alkene class unsaturated alkyl in one or more.
4. Halogen composite flame-proof PC/ABS alloy according to claim 3 is characterized in that, contains methyl and phenyl in the side group of described polyborosiloxane simultaneously.
5. Halogen composite flame-proof PC/ABS alloy according to claim 1 is characterized in that the mol ratio of silicon and boron is (0.3～3) in the described polyborosiloxane: 1, be preferably (0.5～2): 1.
6. Halogen composite flame-proof PC/ABS alloy according to claim 1 is characterized in that described polyborosiloxane is selected weight-average molecular weight≤15000 for use.
7. Halogen composite flame-proof PC/ABS alloy according to claim 2 is characterized in that the Sulfonates fire retardant is perfluoro butyl potassium sulfonate, perfluoro butyl sodium sulfonate or sulfobenzide potassium sulfonate.
8. Halogen composite flame-proof PC/ABS alloy according to claim 2 is characterized in that the preparation method of described fire-retardant master granule is:
Polycarbonate and Sulfonates fire retardant by after the proportioning pre-mixing, were mixed 3 minutes～8 minutes down in 250 ℃～270 ℃ in torque rheometer, make fire-retardant master granule, screw speed is 50r/min～100r/min in the described torque rheometer;
Or, make fire-retardant master granule with in twin screw extruder, melt extruding granulation in 255 ℃～280 ℃ after polycarbonate and the pre-mixing of Sulfonates fire retardant.
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| CN2012102591543A CN102775754A (en) | 2012-07-25 | 2012-07-25 | Halogen-free composite flame retardant poly carbonates (PC)/acrylonitrile butadiene styrene copolymers (ABS) alloy and preparation method thereof |
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| GB2509128A (en) * | 2012-12-20 | 2014-06-25 | Dow Corning | Process for improving fire resistance of an organic polymer |
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| CN109111712A (en) * | 2018-07-17 | 2019-01-01 | 广东聚石化学股份有限公司 | A kind of low smell fire retardation PC material and preparation method thereof |
| CN111205616A (en) * | 2020-02-11 | 2020-05-29 | 上海锦湖日丽塑料有限公司 | Cold-heat-exchange-deformation-resistant halogen-free flame-retardant polycarbonate alloy and preparation method thereof |
| CN113372705A (en) * | 2021-06-16 | 2021-09-10 | 宁波浙铁大风化工有限公司 | Transparent flame-retardant polycarbonate, preparation method thereof and polycarbonate product |
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| CN116875021A (en) * | 2023-08-04 | 2023-10-13 | 山东乐佳达新材料科技有限公司 | PC/ABS alloy material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB2509128A (en) * | 2012-12-20 | 2014-06-25 | Dow Corning | Process for improving fire resistance of an organic polymer |
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| CN111205616A (en) * | 2020-02-11 | 2020-05-29 | 上海锦湖日丽塑料有限公司 | Cold-heat-exchange-deformation-resistant halogen-free flame-retardant polycarbonate alloy and preparation method thereof |
| CN111205616B (en) * | 2020-02-11 | 2022-07-12 | 上海锦湖日丽塑料有限公司 | Cold-heat-exchange-deformation-resistant halogen-free flame-retardant polycarbonate alloy and preparation method thereof |
| CN113372705A (en) * | 2021-06-16 | 2021-09-10 | 宁波浙铁大风化工有限公司 | Transparent flame-retardant polycarbonate, preparation method thereof and polycarbonate product |
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Application publication date: 20121114 |