CN111117186A - Flame-retardant, low-temperature-impact-resistant and high-weather-resistance PC/PBT alloy and preparation method thereof - Google Patents
Flame-retardant, low-temperature-impact-resistant and high-weather-resistance PC/PBT alloy and preparation method thereof Download PDFInfo
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- CN111117186A CN111117186A CN201911346896.8A CN201911346896A CN111117186A CN 111117186 A CN111117186 A CN 111117186A CN 201911346896 A CN201911346896 A CN 201911346896A CN 111117186 A CN111117186 A CN 111117186A
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- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a flame-retardant, low-temperature impact-resistant and high-weather-resistance PC/PBT alloy and a preparation method thereof, wherein the preparation method comprises the following steps: s1, weighing the raw materials; s2, mixing the polycarbonate, the toughening agent, the compatibilizer, the anti-dripping agent, the ester exchange inhibitor, the antioxidant, the lubricant and the light stabilizer at high speed for 3-5 min; s3, mixing the polybutylene terephthalate and the flame retardant at high speed for 2-3 min; and S4, feeding the material obtained in the step S3 into a side feeding cylinder of a co-rotating double-screw extruder, feeding the material obtained in the step S2 into a main feeding cylinder of the co-rotating double-screw extruder, and performing melt extrusion, cooling and granulation to obtain the material. The PC/PBT alloy prepared by the invention has excellent flame retardance, weather resistance and low-temperature impact resistance, can keep better fluidity, has low cost and good comprehensive performance, and has good application prospect.
Description
Technical Field
The invention relates to the technical field of engineering plastics, in particular to a PC/PBT alloy with flame retardance, low-temperature impact resistance and high weather resistance and a preparation method thereof.
Background
Polycarbonate, abbreviated as PC, is a high molecular polymer containing carbonate groups in its molecular chain, and is classified into various types, such as aliphatic, aromatic, aliphatic-aromatic, and the like, according to the structure of the ester groups. PC has the advantage of being rigid and tough at room temperature, but suffers from severe thermal deformation at high temperatures. The disadvantages are stress cracking and high viscosity. Polybutylene terephthalate, PBT for short, belongs to polyester, and is a milky, translucent to opaque, crystalline thermoplastic polyester resin prepared by the process of blending 1, 4-butanediol and terephthalic acid (PTA) or terephthalate (DMT) through condensation. The PBT has the advantages of no influence of temperature on rigidity and small deformation. The PC/PBT alloy keeps the chemical resistance of the crystalline material PBT and the characteristics of easy molding and the like, and has the toughness and the dimensional stability of the amorphous material PC. The product is widely applied to automobile bumpers, automobile handles, electronic components and the like. However, since PC is an amorphous polymer and PBT is a crystalline polymer, PC/PBT belongs to a typical amorphous and crystalline blending system, and has poor interface compatibility, low impact strength, poor flame retardance and poor weather resistance, which greatly limits the application of the PC/PBT.
Because the hydroxyl group at the molecular chain end of Polycarbonate (PC) and the carboxyl group at the molecular chain end of polybutylene terephthalate (PBT) are easy to generate side reactions such as ester exchange and the like in the melt blending process, and the reaction is accelerated in the presence of a flame retardant, how to prepare the flame-retardant weather-resistant PC/PBT alloy with excellent comprehensive performance is always a difficult problem. Therefore, the selection of suitable extrusion processes and auxiliaries is the key to the preparation of high performance PC/PBT alloys.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a PC/PBT alloy with flame retardance, low-temperature impact resistance and high weather resistance and a preparation method thereof.
The invention provides a preparation method of a PC/PBT alloy with flame retardance, low-temperature impact resistance and high weather resistance, which comprises the following steps:
s1, weighing the following raw materials in parts by weight: 45-70 parts of polycarbonate, 15-35 parts of polybutylene terephthalate, 3-6 parts of toughening agent, 1-3 parts of compatibilizer, 5-9 parts of flame retardant, 0.3-0.8 part of anti-dripping agent, 0.1-0.5 part of ester exchange inhibitor, 0.1-0.3 part of antioxidant, 0.1-0.5 part of lubricant and 0.6-1.5 parts of light stabilizer;
s2, mixing the polycarbonate, the toughening agent, the compatibilizer, the anti-dripping agent, the ester exchange inhibitor, the antioxidant, the lubricant and the light stabilizer at high speed for 3-5 min;
s3, mixing the polybutylene terephthalate and the flame retardant at high speed for 2-3 min;
s4, feeding the material obtained in the step S3 into a side feeding cylinder of a co-rotating double-screw extruder, feeding the material obtained in the step S2 into a main feeding cylinder of the co-rotating double-screw extruder, and performing melt extrusion, cooling and granulation to obtain the material
Preferably, the polycarbonate has a density of 1.19 to 1.21g/cm3The melt index at 300 ℃ and 1.2Kg is 8 to 12g/10 min.
Preferably, the polybutylene terephthalate has a density of 1.29 to 1.32g/cm3The intrinsic viscosity is 0.9-1.1.
Preferably, the toughening agent is one or more of polyolefin elastomer (POE), ethylene-methyl acrylate (EMA), ethylene-methyl acrylate copolymer and methyl methacrylate-butadiene-styrene terpolymer (MBS) with a core-shell structure.
Preferably, the compatibilizer is one or more of ethylene-butyl acrylate-glycidyl methacrylate ternary random copolymer (EBA-g-GMA), ethylene-octene-glycidyl methacrylate ternary random copolymer (POE-g-GMA) and styrene-acrylonitrile-glycidyl methacrylate ternary random copolymer.
Preferably, the flame retardant consists of antimony trioxide and an organic flame retardant, wherein the organic flame retardant is one or more of tetrabromobisphenol A-tetrabromobisphenol A epoxy propyl ether copolymer, 1, 2-bis (2,3,4,5, 6-pentabromophenyl) ethane, 2,4, 6-tris (2,4, 6-tribromophenoxy) -1,3, 5-triazine and isopropyl phenol phosphate.
Preferably, the ester exchange inhibitor is one or more of pentaerythritol diphosphite, monododecyl phosphate, didodecyl phosphate and octadecyl phosphite.
Preferably, the antioxidant consists of a main antioxidant and an auxiliary antioxidant, wherein the main antioxidant is antioxidant 1076 or antioxidant 1010, and the auxiliary antioxidant is antioxidant 168, antioxidant 626 or antioxidant 412S; the light stabilizer consists of a benzotriazole ultraviolet absorber and a hindered amine light stabilizer.
Preferably, the anti-dripping agent is polytetrafluoroethylene powder.
Preferably, the lubricant is pentaerythritol stearate.
Preferably, the granulation temperature of the double-screw extruder is 230-250 ℃, the pressure of the vacuum pump is 0.05-0.07MPa, and the rotating speed is 350-450 r/min.
The PC/PBT alloy with flame retardance, low-temperature impact resistance and high weather resistance is prepared by the preparation method.
The invention has the following beneficial effects:
compared with the prior art, in order to prevent the ester exchange reaction between PC and PBT and the decomposition of PC caused by the flame retardant, the invention adopts the process of feeding the mixture of polybutylene terephthalate and the flame retardant into the feeding cylinder from the side, and selects the light stabilizer, the compatilizer and other auxiliaries to blend to prepare the PC/PBT alloy, which has excellent flame retardance, weather resistance and low-temperature impact resistance, can keep better fluidity, and has low cost, good comprehensive performance and good application prospect.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A flame-retardant, low-temperature impact-resistant and high-weather-resistance PC/PBT alloy comprises the following raw materials in parts by weight:
70 parts of polycarbonate, 16 parts of polybutylene terephthalate, 5 parts of toughening agent, 1 part of compatibilizer, 6 parts of flame retardant, 0.5 part of anti-dripping agent, 0.15 part of ester exchange inhibitor, 0.15 part of antioxidant, 0.3 part of lubricant and 0.9 part of light stabilizer.
Wherein the polycarbonate has a density of 1.19g/cm3At 300 deg.C and 1.2KgThe melt index measured according to ASTM D1238 is 8g/10 min; the density of polybutylene terephthalate is 1.29g/cm3The intrinsic viscosity was 0.9.
The flame retardant is a mixture of tetrabromobisphenol A-tetrabromobisphenol A epoxy propyl ether copolymer and antimony trioxide in a weight ratio of 4:1, the anti-dripping agent is polytetrafluoroethylene powder, the ester exchange inhibitor is pentaerythritol diphosphite, the antioxidant is a mixture of antioxidant 1010 and antioxidant 168 in a weight ratio of 1:1, the lubricant is pentaerythritol stearate, and the light stabilizer is a mixture of benzotriazole ultraviolet absorbent and hindered amine light stabilizer in a weight ratio of 2: 1.
The preparation method comprises the following steps:
s1, mixing the polycarbonate, the toughening agent, the compatibilizer, the anti-dripping agent, the ester exchange inhibitor, the antioxidant, the lubricant and the light stabilizer at high speed for 3 min;
s2, mixing the polybutylene terephthalate and the flame retardant for 2min at a high speed;
and S3, feeding the material obtained in the step S2 into a side feeding cylinder of a co-rotating double-screw extruder, feeding the material obtained in the step S1 into a main feeding cylinder of the co-rotating double-screw extruder, and performing melt extrusion, cooling and granulation to obtain the material.
Wherein the granulation temperature of the double-screw extruder is 230 ℃, the pressure of a vacuum pump is 0.06MPa, and the rotating speed is 400 r/min.
Example 2
A flame-retardant, low-temperature impact-resistant and high-weather-resistance PC/PBT alloy comprises the following raw materials in parts by weight:
polycarbonate 61, polybutylene terephthalate 25, toughening agent 4, compatibilizer 1, flame retardant 7, anti-dripping agent 0.6, ester exchange inhibitor 0.2, antioxidant 0.2, lubricant 0.3 and light stabilizer 0.7.
Wherein the polycarbonate has a density of 1.21g/cm3The melt index measured according to ASTM D1238 at 300 ℃ under 1.2Kg is 12g/10 min; density of polybutylene terephthalateIs 1.32g/cm3The intrinsic viscosity was 1.1.
The flame retardant is a mixture of tetrabromobisphenol A-tetrabromobisphenol A epoxy propyl ether copolymer and antimony trioxide in a weight ratio of 4:1, the anti-dripping agent is polytetrafluoroethylene powder, the ester exchange inhibitor is pentaerythritol diphosphite, the antioxidant is a mixture of antioxidant 1010 and antioxidant 168 in a weight ratio of 1:1, the lubricant is pentaerythritol stearate, and the light stabilizer is a mixture of benzotriazole ultraviolet absorbent and hindered amine light stabilizer in a weight ratio of 2: 1.
The preparation method comprises the following steps:
s1, mixing the polycarbonate, the toughening agent, the compatibilizer, the anti-dripping agent, the ester exchange inhibitor, the antioxidant, the lubricant and the light stabilizer at high speed for 4 min;
s2, mixing the polybutylene terephthalate and the flame retardant at a high speed for 2.5 min;
and S3, feeding the material obtained in the step S2 into a side feeding cylinder of a co-rotating double-screw extruder, feeding the material obtained in the step S1 into a main feeding cylinder of the co-rotating double-screw extruder, and performing melt extrusion, cooling and granulation to obtain the material.
Wherein the granulation temperature of the double-screw extruder is 250 ℃, the pressure of a vacuum pump is 0.07MPa, and the rotating speed is 450 r/min.
Example 3
A flame-retardant, low-temperature impact-resistant and high-weather-resistance PC/PBT alloy comprises the following raw materials in parts by weight:
polycarbonate 49, polybutylene terephthalate 35, toughening agent 4, compatibilizer 1, flame retardant 9, anti-dripping agent 0.6, ester exchange inhibitor 0.2, antioxidant 0.2, lubricant 0.3 and light stabilizer 0.7.
Wherein the polycarbonate has a density of 1.2g/cm3The melt index measured according to ASTM D1238 at 300 ℃ under 1.2Kg is 10g/10 min; the density of polybutylene terephthalate is 1.3g/cm3The intrinsic viscosity was 1.0.
The flame retardant is a mixture of tetrabromobisphenol A-tetrabromobisphenol A epoxy propyl ether copolymer and antimony trioxide in a weight ratio of 4:1, the anti-dripping agent is polytetrafluoroethylene powder, the ester exchange inhibitor is pentaerythritol diphosphite, the antioxidant is a mixture of antioxidant 1010 and antioxidant 168 in a weight ratio of 1:1, the lubricant is pentaerythritol stearate, and the light stabilizer is a mixture of benzotriazole ultraviolet absorbent and hindered amine light stabilizer in a weight ratio of 2: 1.
The preparation method comprises the following steps:
s1, mixing polycarbonate, a toughening agent, a compatibilizer, an anti-dripping agent, an ester exchange inhibitor, an antioxidant, a lubricant and a light stabilizer at high speed for 5 min;
s2, mixing the polybutylene terephthalate and the flame retardant for 3min at a high speed;
and S3, feeding the material obtained in the step S2 into a side feeding cylinder of a co-rotating double-screw extruder, feeding the material obtained in the step S1 into a main feeding cylinder of the co-rotating double-screw extruder, and performing melt extrusion, cooling and granulation to obtain the material.
Wherein the granulation temperature of the double-screw extruder is 240 ℃, the pressure of a vacuum pump is 0.05MPa, and the rotating speed is 350 r/min.
Comparative example 1
A flame-retardant, low-temperature impact-resistant and high-weather-resistance PC/PBT alloy comprises the following raw materials in parts by weight:
polycarbonate 49, polybutylene terephthalate 35, toughening agent 4, flame retardant 9, anti-dripping agent 0.6, ester exchange inhibitor 0.2, antioxidant 0.2 and lubricant 0.3.
Wherein the polycarbonate has a density of 1.2g/cm3A melt index of 10g/10min measured according to ASTM D1238 at 300 ℃ under 1.2 Kg; the density of polybutylene terephthalate is 1.3g/cm3The intrinsic viscosity was 1.0.
The flame retardant is a mixture of tetrabromobisphenol A-tetrabromobisphenol A epoxy propyl ether copolymer and antimony trioxide in a weight ratio of 4:1, the anti-dripping agent is polytetrafluoroethylene powder, the ester exchange inhibitor is pentaerythritol diphosphite, the antioxidant is a mixture of antioxidant 1010 and antioxidant 168 in a weight ratio of 1:1, the lubricant is pentaerythritol stearate, and the light stabilizer is a mixture of benzotriazole ultraviolet absorbent and hindered amine light stabilizer in a weight ratio of 2: 1.
The preparation method comprises the following steps:
s1, mixing the polycarbonate, the toughening agent, the anti-dripping agent, the ester exchange inhibitor, the antioxidant and the lubricant at high speed for 5 min;
s2, mixing the polybutylene terephthalate and the flame retardant for 3min at a high speed;
and S3, feeding the material obtained in the step S2 into a side feeding cylinder of a co-rotating double-screw extruder, feeding the material obtained in the step S1 into a main feeding cylinder of the co-rotating double-screw extruder, and performing melt extrusion, cooling and granulation to obtain the material.
Wherein the granulation temperature of the double-screw extruder is 240 ℃, the pressure of a vacuum pump is 0.05MPa, and the rotating speed is 350 r/min.
Comparative example 2
A flame-retardant, low-temperature impact-resistant and high-weather-resistance PC/PBT alloy comprises the following raw materials in parts by weight:
polycarbonate 49, polybutylene terephthalate 35, toughening agent 4, compatibilizer 1, flame retardant 9, anti-dripping agent 0.6, ester exchange inhibitor 0.2, antioxidant 0.2, lubricant 0.3 and light stabilizer 0.7.
Wherein the polycarbonate has a density of 1.2g/cm2A melt index of 10g/10min measured according to ASTM D1238 at 300 ℃ under 1.2 Kg; the density of polybutylene terephthalate is 1.3g/cm2The intrinsic viscosity was 1.0.
The flame retardant is a mixture of tetrabromobisphenol A-tetrabromobisphenol A epoxy propyl ether copolymer and antimony trioxide in a weight ratio of 4:1, the anti-dripping agent is polytetrafluoroethylene powder, the ester exchange inhibitor is pentaerythritol diphosphite, the antioxidant is a mixture of antioxidant 1010 and antioxidant 168 in a weight ratio of 1:1, the lubricant is pentaerythritol stearate, and the light stabilizer is a mixture of benzotriazole ultraviolet absorbent and hindered amine light stabilizer in a weight ratio of 2: 1.
The preparation method comprises the following steps:
s1, mixing polycarbonate, polybutylene terephthalate, a toughening agent, a compatibilizer, a flame retardant, an anti-dripping agent, an ester exchange inhibitor, an antioxidant, a lubricant and a light stabilizer at high speed for 5 min;
and S2, putting the material obtained in the step S1 into a main feeding cylinder of a co-rotating double-screw extruder, and performing melt extrusion, cooling and granulation to obtain the material.
Wherein the granulation temperature of the double-screw extruder is 240 ℃, the pressure of a vacuum pump is 0.05MPa, and the rotating speed is 350 r/min.
The PC/PBT alloys obtained in examples 1-3 and comparative examples 1-2 were subjected to performance tests, and the results are shown in Table 1:
TABLE 1 raw Material composition of PC/PBT alloy and Performance test results
As can be seen from the table, the PC/PBT alloy prepared by the material formula and the process has excellent impact resistance, and the normal temperature impact is 50KJ/m2The flame retardant with the thickness of 1.6mm can reach the UL V0 grade, and has good weather resistance, no obvious yellowing after being stored for 500 hours at 80 ℃, and the color difference within 5.0 after being irradiated by ultraviolet for 300 hours.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The preparation method of the PC/PBT alloy with flame retardance, low-temperature impact resistance and high weather resistance is characterized by comprising the following steps of:
s1, weighing the following raw materials in parts by weight: 45-70 parts of polycarbonate, 15-35 parts of polybutylene terephthalate, 3-6 parts of toughening agent, 1-3 parts of compatibilizer, 5-9 parts of flame retardant, 0.3-0.8 part of anti-dripping agent, 0.1-0.5 part of ester exchange inhibitor, 0.1-0.3 part of antioxidant, 0.1-0.5 part of lubricant and 0.6-1.5 parts of light stabilizer;
s2, mixing the polycarbonate, the toughening agent, the compatibilizer, the anti-dripping agent, the ester exchange inhibitor, the antioxidant, the lubricant and the light stabilizer at high speed for 3-5 min;
s3, mixing the polybutylene terephthalate and the flame retardant at high speed for 2-3 min;
and S4, feeding the material obtained in the step S3 into a side feeding cylinder of a co-rotating double-screw extruder, feeding the material obtained in the step S2 into a main feeding cylinder of the co-rotating double-screw extruder, and performing melt extrusion, cooling and granulation to obtain the material.
2. The method of claim 1, wherein the polycarbonate has a density of 1.19-1.21g/cm3The melt index at 300 ℃ and 1.2Kg is 8 to 12g/10 min.
3. The method for preparing a PC/PBT alloy having flame retardancy, low temperature impact resistance and high weather resistance according to claim 1 or 2, wherein the polybutylene terephthalate has a density of 1.29 to 1.32g/cm3The intrinsic viscosity is 0.9-1.1.
4. The preparation method of the PC/PBT alloy with flame retardance, low-temperature impact resistance and high weather resistance according to any one of claims 1 to 3, wherein the toughening agent is one or more of a polyolefin elastomer, ethylene-methacrylate, an ethylene-methyl acrylate copolymer and a methyl methacrylate-butadiene-styrene terpolymer with a core-shell structure.
5. The method for preparing the PC/PBT alloy with flame retardance, low-temperature impact resistance and high weather resistance according to any one of claims 1 to 4, wherein the compatibilizer is one or more of ethylene-butyl acrylate-glycidyl methacrylate ternary random copolymer, ethylene-octene-glycidyl methacrylate ternary random copolymer and styrene-acrylonitrile-glycidyl methacrylate ternary random copolymer.
6. The method for preparing a flame retardant, low temperature impact resistant and highly weather resistant PC/PBT alloy according to any of claims 1 to 5, wherein the flame retardant is composed of antimony trioxide and an organic flame retardant which is one or more of tetrabromobisphenol A-tetrabromobisphenol A glycidyl ether copolymer, 1, 2-bis (2,3,4,5, 6-pentabromophenyl) ethane, 2,4, 6-tris (2,4, 6-tribromophenoxy) -1,3, 5-triazine, isopropylphenol phosphate.
7. The method for preparing a flame retardant, low temperature impact resistant and high weather resistant PC/PBT alloy according to any one of claims 1 to 6, wherein the ester exchange inhibitor is one or more of pentaerythritol diphosphite, monododecyl phosphate, didodecyl phosphate, octadecyl phosphite.
8. The method for preparing the PC/PBT alloy with flame retardance, low-temperature impact resistance and high weather resistance according to any one of claims 1 to 7, wherein the antioxidant consists of a primary antioxidant 1076 or 1010 and a secondary antioxidant 168, 626 or 412S; the light stabilizer consists of a benzotriazole ultraviolet absorber and a hindered amine light stabilizer.
9. The method for preparing the PC/PBT alloy with flame retardance, low-temperature impact resistance and high weather resistance according to any one of claims 1 to 8, wherein the granulation temperature of the double-screw extruder is 230-250 ℃, the pressure of the vacuum pump is 0.05-0.07MPa, and the rotating speed is 350-450 r/min.
10. A PC/PBT alloy that is flame retardant, resistant to low temperature impact and highly weather resistant, characterized by being produced by the production method of any one of claims 1-9.
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| CN112724633A (en) * | 2020-12-25 | 2021-04-30 | 中广核高新核材科技（苏州）有限公司 | Cold-resistant flame-retardant PC/PBT material and preparation method thereof |
| CN112795164A (en) * | 2021-01-14 | 2021-05-14 | 万华化学(四川)有限公司 | PC/PBA alloy material and preparation method thereof |
| CN113637310A (en) * | 2021-08-17 | 2021-11-12 | 金发科技股份有限公司 | Polycarbonate/polyester alloy composition with long-term thermal oxidation stability and preparation method and application thereof |
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| CN114031922A (en) * | 2021-12-15 | 2022-02-11 | 太仓市华鼎塑料有限公司 | Low-temperature impact resistant PCPBT alloy material for vehicles and preparation method thereof |
| CN114591607A (en) * | 2022-03-17 | 2022-06-07 | 江苏金发科技新材料有限公司 | PBT composition and preparation method and application thereof |
| CN115160759A (en) * | 2022-07-26 | 2022-10-11 | 四川长虹智能制造技术有限公司 | Flame-retardant and chemical-resistant PC/PBT alloy material and preparation method and application thereof |
| CN115895224A (en) * | 2022-10-19 | 2023-04-04 | 湖北合聚新材料有限公司 | PBT/PC alloy and preparation method and device thereof |
| WO2023055099A1 (en) * | 2021-09-30 | 2023-04-06 | (주) 엘지화학 | Thermoplastic resin and molded article made thereof |
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