CN115627059B - PC/PET alloy material and preparation method and application thereof - Google Patents
PC/PET alloy material and preparation method and application thereof Download PDFInfo
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- CN115627059B CN115627059B CN202211181955.2A CN202211181955A CN115627059B CN 115627059 B CN115627059 B CN 115627059B CN 202211181955 A CN202211181955 A CN 202211181955A CN 115627059 B CN115627059 B CN 115627059B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60R—VEHICLES, VEHICLE FITTINGS, OR VEHICLE PARTS, NOT OTHERWISE PROVIDED FOR
- B60R13/00—Elements for body-finishing, identifying, or decorating; Arrangements or adaptations for advertising purposes
- B60R13/04—External Ornamental or guard strips; Ornamental inscriptive devices thereon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/324—Alkali metal phosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
Abstract
The invention discloses a PC/PET alloy material, a preparation method and application thereof, wherein the PC/PET alloy material comprises the following components in parts by weight: 60-75 parts of polycarbonate resin; 20-35 parts of polyethylene terephthalate; 3-8 parts of compound compatibilizer and flexibilizer; 0.3-2 parts of functionalized carbon nano tube; 0.1-0.4 part of transesterification inhibitor; 0.3-0.8 part of other processing aids. The PC/PET alloy material provided by the invention has high strength, high impact resistance and high thermal stability, and can be suitable for products of automobile exterior trimming parts such as bumpers, grids, spoilers and the like.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a PC/PET alloy material, a preparation method and application thereof.
Background
The Polycarbonate (PC) is a colorless transparent amorphous polymer, and has high impact resistance, heat resistance, transparency and high dimensional stability due to the special molecular structure and the alternating arrangement of flexible ester groups and rigid benzene rings in the molecular chain, and has wide application in the market. However, PC resins also suffer from poor processability, poor stress crack resistance and poor solvent resistance, and impact properties are susceptible to chipping, also limiting their use to a great extent. Polyethylene terephthalate (PET) is used as another engineering plastic and has the advantages of excellent processing fluidity, outstanding chemical resistance, low stress, low price and the like. However, they have disadvantages such as poor impact properties and long molding cycles. The PC/PET alloy material prepared by melt blending the two plastics combines the advantages and disadvantages of the two plastics, and can make up the respective defects. However, although PC and PET are both linear aromatic polyesters, the chemical results are similar, the PC/PET alloy material obtained by blending the two is a typical amorphous/crystalline polymer system, the interfacial bonding strength is poor, the impact strength cannot be effectively improved, that is, the alloy material obtained by simply melt blending PC and PET cannot meet the requirements of toughness of alloy materials in various fields. For this reason, toughening modification is required in PC/PET alloy systems. At present, the PC/PET alloy system is toughened by mainly adopting a reactive compatibilizer or an elastomer, but the method can improve the impact resistance of the material and obviously reduce the strength and rigidity of the material. In addition, because of the existence of the ester group structure in the PC and PET molecular chains, transesterification reaction is easy to occur during the high-temperature melt extrusion processing process, the crystallization and melting behavior of PET are affected, and the PC/PET alloy material has extremely negative effects on the performance and the molding stability of the PC/PET alloy material.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a PC/PET alloy material, and a preparation method and application thereof. The PC/PET alloy material provided by the invention not only has high strength and high shock resistance, but also has excellent heat stability.
The method is realized by the following technical scheme:
the PC/PET alloy material comprises the following components in parts by weight:
further, the polycarbonate resin has a melt index of 3 to 20g/10min under the condition of 300 ℃/1.2kg, more preferably, the polycarbonate resin has a melt index of 8 to 15g/10min under the condition of 300 ℃/1.2kg, as tested in accordance with ISO 1133-1-2011 standard. If the melt index of the polycarbonate resin is too low, the viscosity is high, and the polycarbonate resin is not easy to process and form; if the melt index of the polycarbonate resin is too high, namely the viscosity is low, the heat-resistant stability of the material is poor, and the heat-resistant stability and mechanical properties of the material are affected.
Further, the polyethylene terephthalate has a melt index of 10-35g/10min at 270 ℃/1.2kg, more preferably, the polyethylene terephthalate has a melt index of 19-25g/10min at 270 ℃/1.2kg, as tested in accordance with ISO 1133-1-2011.
Further, the compound compatibilizer and toughening agent is a methyl methacrylate-butadiene-styrene copolymer and an ethylene-butyl acrylate-glycidyl methacrylate copolymer.
Further, the weight ratio of the methyl methacrylate-butadiene-styrene copolymer to the ethylene-butyl acrylate-glycidyl methacrylate copolymer is 1:1-3:1, preferably, the weight ratio of the methyl methacrylate-butadiene-styrene copolymer to the ethylene-butyl acrylate-glycidyl methacrylate copolymer is 2:1. If the weight ratio of the methyl methacrylate-butadiene-styrene copolymer to the ethylene-butyl acrylate-glycidyl methacrylate copolymer is too high, the ethylene-butyl acrylate-glycidyl methacrylate content is low, the PET end capping effect is poor, the risk of transesterification reaction is increased, and the heat-resistant stability and mechanical properties of the final material are affected. If the ratio of the two is too low, namely the content of ethylene-butyl acrylate-glycidyl methacrylate is high, the rigidity of the alloy material is reduced, and the thermal stability of the material is also poor.
Further, the functionalized carbon nanotubes are carboxylated carbon nanotubes, wherein the carboxyl content is 1-2.5wt%. If the carboxylation content of the functionalized carbon nano tube is too low, the reaction efficiency with the compound compatibilization and toughening agent in the system is low, and the effect of strengthening and toughening and improving the thermal stability of the functionalized carbon nano tube is affected. Meanwhile, the PC and PET cannot be effectively blocked, and the risk of side reactions is increased. The hydroxylation content is too high, the carbon nano tube structure is seriously damaged, the performance of the carbon nano tube is influenced, and the effects of reinforcing, toughening and improving the thermal stability of the carbon nano tube are further influenced.
The preparation method of the carboxylated carbon nano tube comprises the following steps:
placing the carbon nano tube in mixed acid (the volume ratio of concentrated sulfuric acid to nitric acid is 3:1), carrying out ultrasonic treatment for 3-5h, and then refluxing at 80 ℃ for 1-2h; then diluted with deionized water and left to settle for 24 hours to give a yellow supernatant. After removing the supernatant, the lower layer carbon nanotube dispersion is subjected to suction filtration by using a polyvinylidene fluoride micro-filtration membrane with the pore diameter of 0.2 mu m, repeatedly washed by deionized water until the solution is neutral, and dried at the temperature of 100 ℃ to obtain the carboxylated carbon nanotubes. Wherein the carboxyl content is calculated by an acid-base titration method principle.
Specifically, the transesterification inhibitor is sodium dihydrogen phosphate.
Further, the other processing aid is at least one of an antioxidant and a lubricant.
The antioxidant can be one or more of hindered phenol antioxidants or phosphite antioxidants, such as antioxidant 1010 and antioxidant 168.
The lubricant may be one or more of a silicone-based lubricant or a pentaerythritol stearate-based lubricant.
The invention also provides a preparation method of the PC/PET alloy material, which comprises the following steps:
s1: weighing the components according to the proportion;
s2: melting, extruding and granulating polyethylene terephthalate (PET) and the functionalized carbon nano tube by an extruder to prepare polyethylene terephthalate/carbon nano tube granules;
s3: and (2) premixing, melt extrusion and granulating the polyethylene terephthalate/carbon nano tube granules, polycarbonate, the compound compatibilizer and toughening agent and other processing aids which are prepared in the step (S2) to obtain the PC/PET alloy material.
Further, in steps S2 and S3, the process parameters of melt extrusion are: the temperature of the feeding section is 190-220 ℃, the temperature of the plasticizing section is 230-260 ℃, the temperature of the homogenizing section is 250-270 ℃, and the screw rotation speed is 300-600rpm.
The invention also provides application of the PC/PET alloy material in preparing automobile exterior trimming parts, such as products of bumpers, gratings, spoilers and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. through the optimal design of the formula, in the weight parts of PC and PET respectively selected in the invention, the PC matrix is a continuous phase, and the methyl methacrylate-butadiene-styrene copolymer in the compound compatibilizer-toughening agent can be selectively and uniformly dispersed in the PC continuous phase, so that a good toughening effect is achieved. In addition, the epoxy functional group of the ethylene-butyl acrylate-glycidyl methacrylate copolymer in the compound compatibilizer-toughening agent can be subjected to chemical reaction with the end group of PET so as to be distributed at the phase interface of PC/PET, so that the compatibility of the interface between PC and PET is improved, the synergistic effect of the epoxy functional group and the transesterification inhibitor is achieved, the degree of transesterification reaction is reduced, and the melt processing stability is improved while the toughening effect is realized. Finally, carboxylated carbon nanotubes are added into the alloy system, and the carboxyl groups of the carboxylated carbon nanotubes are subjected to end capping with PC and PET end groups, so that side reactions such as transesterification and the like of the alloy material in the high-temperature extrusion and subsequent injection molding processes are further reduced, and the effect of high thermal stability is realized.
2. According to the invention, through the optimization design of the process, PET is firstly melt-blended with the functionalized carbon nano tube and then blended with PC, the compound compatibilizer and toughening agent and other auxiliary agents, on one hand, the functionalized carbon nano tube can increase the melt viscosity of the PET, so that the viscosity difference between the PET and PC resin is reduced, and the PET is well dispersed in a PC continuous phase. On the other hand, most of the functionalized carbon nanotubes can be dispersed in the PET resin to play a role in heterogeneous nucleation, so that the crystallization performance of the PET material is reserved; meanwhile, part of the functionalized carbon nano tube reacts with the epoxy functional group of the ethylene-butyl acrylate-glycidyl methacrylate copolymer in the compound compatibilizer-toughening agent, so that a bridge function is achieved, the interface function of PET and PC is further improved, and the reinforcing and toughening effects are realized.
3. The synergistic optimization of the combination of the formula and the process is the key for preparing the PC/PET alloy material with high strength, high impact resistance and high thermal stability. The PC/PET alloy material prepared by the invention has the tensile strength of 54.2-60.7MPa, the bending strength of 80.4-88.9MPa, the bending modulus of 2106-2387MPa and the notch impact strength of 47.8-67.3kJ/m 2 The heat distortion temperature is 98-107 ℃, and the melt index change rate is 15.4-23.5%.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
< preparation of examples and comparative examples >
The raw materials used in the examples and comparative examples of the present invention are all commercially available, but are not limited to these materials:
polycarbonate resin a: the melt index under the conditions of 300 ℃/1.2kg is 10g/10min, and the brand PC 2100 is purchased from Wanhua Shandong;
polycarbonate resin B: the melt index under the conditions of 300 ℃/1.2kg is 20g/10min, and the brand PC 2220 is purchased from Wanhua Shandong;
polycarbonate resin C: the melt index under the conditions of 300 ℃/1.2kg is 35g/10min, and the brand PC H-3000F is purchased from Mitsubishi Japanese;
polycarbonate resin D: the melt index at 300 ℃/1.2kg was 3g/10min, brand PC1300 03NP, available from LG chemistry;
polyethylene terephthalate a: the melt index under the condition of 270 ℃/1.2kg is 19g/min, and the brand PET BG80 is purchased from medium petrochemical instrumentation chemical fiber;
polyethylene terephthalate B: the melt index under the conditions of 270 ℃/1.2kg is 35g/min, the brand PET FG600 is purchased from medium petrochemical instrumentation chemical fiber;
methyl methacrylate-butadiene-styrene copolymer: brand MBS EM500, purchased from LG chemistry;
ethylene-butyl acrylate-glycidyl methacrylate copolymer: brand AX8700, available from alcima, france;
functionalized carbon nanotubes a: the carboxyl content is 1.5 weight percent, and the preparation is self-made;
functionalized carbon nanotubes B: the carboxyl content is 1 weight percent, and the preparation is self-made;
functionalized carbon nanotubes C: the carboxyl content is 2.5 weight percent, and the preparation is self-made;
functionalized carbon nanotubes D: the carboxyl content is 0.6 weight percent, and the product is self-made;
functionalized carbon nanotubes E: the carboxyl content is 2.8 weight percent, and the product is self-made;
carbon nanotubes: brand NTP3021, available from Shenzhen nano harbor Co., ltd;
transesterification inhibitors: sodium dihydrogen phosphate, available from su zhou rich chemical engineering, inc;
antioxidant A: pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (i.e., antioxidant 1010), commercially available, and the same commercially available product was used in parallel experiments;
and (3) an antioxidant B: phosphite antioxidants, commercially available, were used in parallel experiments using the same commercial product;
and (3) a lubricant: pentaerythritol stearate, commercially available, was used in parallel experiments using the same commercially available product.
The preparation methods of inventive examples 1-15 and comparative examples 1-8 are as follows:
s1, weighing the components according to the proportions of the table 1, the table 2 and the table 5;
s2: melting and blending polyethylene terephthalate (PET) and the functionalized carbon nano tube by a double screw extruder, extruding and granulating to obtain polyethylene terephthalate/carbon nano tube granules, wherein the melting extrusion molding parameters are as follows: the temperature of the feeding section is 200 ℃, the temperature of the plasticizing section is 250 ℃, the temperature of the homogenizing section is 270 ℃, and the rotation speed of the screw is 400rpm;
s3: premixing, melt extrusion and granulating the polyethylene terephthalate/carbon nano tube granules, polycarbonate, the compound compatibilizer and flexibilizer and other processing aids prepared in the step S2 to obtain a PC/PET alloy material, wherein the melt extrusion molding parameters are as follows: the temperature of the feeding section was 200 ℃, the temperature of the plasticizing section was 250 ℃, the temperature of the homogenizing section was 270 ℃, and the screw rotation was 400rpm.
The preparation method of comparative example 9 is as follows:
s1: weighing the components according to the formula of the example 1;
s2: and premixing polyethylene terephthalate (PET), a functionalized carbon nano tube, polycarbonate, a compound compatibilizer and flexibilizer and other processing aids, and carrying out melt extrusion and granulation to obtain the PC/PET alloy material. The parameters of melt extrusion molding are as follows: the temperature of the feeding section was 200 ℃, the temperature of the plasticizing section was 250 ℃, the temperature of the homogenizing section was 270 ℃, and the screw rotation was 400rpm.
In the present specification, "parts" means "parts by weight" unless specifically stated otherwise.
< test Standard >
The performance test criteria for each of the examples and comparative examples of the present invention are as follows:
tensile strength: the test is carried out according to ISO 527-2-2012, and the test speed is 50mm/min;
flexural strength and flexural modulus: according to ISO 178-2019, the test speed is 2mm/min;
notched impact strength: according to ISO 179-1-2010 standard;
heat distortion temperature: according to ISO 75-2-2013 standard, adopting A method;
high thermal stability: after 5min and 15min residence in the melt flow tester, the melt flow rate was tested and the rate of change of the melt finger after 5min and 15min residence was calculated. The smaller the melt index change rate is, the better the thermal stability of the alloy material is.
TABLE 1 EXAMPLES 1 to 8 formulations
TABLE 2 EXAMPLES 9 to 15 formulations
TABLE 3 Performance test results for examples 1-8
TABLE 4 test results for examples 9-15
TABLE 5 formulation of comparative examples 1-9
TABLE 6 Performance test results for comparative examples 1-9
As can be seen from the above examples and comparative examples, the PC/PET alloy material prepared by adding the functionalized carbon nanotubes, the methyl methacrylate-butadiene-styrene copolymer and the ethylene-butyl acrylate-glycidyl methacrylate copolymer to compound and adopting a two-step preparation process has the characteristics of high strength, high impact resistance and high thermal stability, and is very suitable for automobile exterior trimming parts such as bumpers, grids, spoilers and the like.
Comparative example 1 compared to example 1, comparative example 1 was free of added functionalized carbon nanotubes, resulting in comparative example 1 having low strength, poor impact resistance and poor thermal stability;
comparative examples 2 and 3 compared with example 3, comparative example 2 was not added with ethylene-butyl acrylate-glycidyl methacrylate copolymer, comparative example 3 was not added with methyl methacrylate-butadiene-styrene copolymer, i.e., both were not compounded with methyl methacrylate-butadiene-styrene copolymer and ethylene-butyl acrylate-glycidyl methacrylate copolymer, resulting in that the balance of properties of strength, impact resistance and thermal stability of comparative examples 2 and 3 could not be achieved.
The comparative examples 4 and 5 have an out-of-range fraction of the functionalized carbon nanotubes compared to example 1, resulting in deterioration of the strength, flexural modulus, impact resistance and thermal stability of the comparative examples 4 and 5.
The comparative examples 6 and 7 were compared with example 1, and the addition amount of the compound compatibilizer-toughening agent was out of range, resulting in poor strength, flexural modulus, impact resistance and thermal stability of the comparative examples 6 and 7.
Comparative example 8 uses a general carbon nanotube, and comparative example 8 does not achieve high strength, high impact resistance and good thermal stability, as compared with example 1.
Comparative example 9 and example 1, both of which use the same formulation, are different in that comparative example 9 does not use the specific preparation method provided by the present invention, resulting in poor performance of comparative example 9.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (9)
1. The PC/PET alloy material is characterized by comprising the following components in parts by weight:
the compound compatibilizer and toughening agent is a methyl methacrylate-butadiene-styrene copolymer and an ethylene-butyl acrylate-glycidyl methacrylate copolymer;
the preparation method of the PC/PET alloy material comprises the following steps:
s1: weighing the components according to the proportion;
s2: melting and extruding polyethylene terephthalate and carboxylated carbon nano tubes through an extruder, and granulating to obtain polyethylene terephthalate/carbon nano tube granules;
s3: and (2) premixing, melt extrusion and granulating the polyethylene terephthalate/carbon nano tube granules, polycarbonate, the compound compatibilizer and toughening agent and other processing aids which are prepared in the step (S2) to obtain the PC/PET alloy material.
2. The PC/PET alloy material of claim 1, wherein the polycarbonate resin has a melt index of 3-20g/min at 300 ℃/1.2 kg.
3. The PC/PET alloy material of claim 1, wherein the polyethylene terephthalate has a melt index of 10-35g/min at 270 ℃/1.2 kg.
4. The PC/PET alloy material of claim 1, wherein the weight ratio of methyl methacrylate-butadiene-styrene copolymer to ethylene-butyl acrylate-glycidyl methacrylate copolymer is 1:1 to 3:1.
5. The PC/PET alloy material according to claim 1, wherein the carboxyl group content in the carboxylated carbon nanotubes is 1-2.5wt%.
6. The PC/PET alloy material of claim 1, wherein the transesterification inhibitor is sodium dihydrogen phosphate.
7. The PC/PET alloy material of claim 1, wherein the other processing aid is at least one of an antioxidant and a lubricant.
8. A method for producing a PC/PET alloy material according to any one of claims 1 to 7, comprising the steps of:
s1: weighing the components according to the proportion;
s2: melting and extruding polyethylene terephthalate and the functionalized carbon nano tube through an extruder, and granulating to obtain polyethylene terephthalate/carbon nano tube granules;
s3: and (2) premixing, melt extrusion and granulating the polyethylene terephthalate/carbon nano tube granules, polycarbonate, the compound compatibilizer and toughening agent and other processing aids which are prepared in the step (S2) to obtain the PC/PET alloy material.
9. Use of the PC/PET alloy material according to any one of claims 1 to 7 for the production of automotive exterior trim parts.
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