CN115627059A - 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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- CN115627059A CN115627059A CN202211181955.2A CN202211181955A CN115627059A CN 115627059 A CN115627059 A CN 115627059A CN 202211181955 A CN202211181955 A CN 202211181955A CN 115627059 A CN115627059 A CN 115627059A
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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
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- 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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- 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
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Abstract
The invention discloses a PC/PET alloy material and 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 glycol terephthalate; 3-8 parts of a compound compatibilization toughening agent; 0.3-2 parts of functionalized carbon nano tubes; 0.1-0.4 part of ester exchange inhibitor; 0.3 to 0.8 portion 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 automobile exterior trimming parts such as bumpers, grids, spoilers and other products.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a PC/PET alloy material and a preparation method and application thereof.
Background
Polycarbonate (PC) is a colorless and transparent amorphous polymer, and has high impact resistance, heat resistance, transparency and good dimensional stability due to the special molecular structure and the alternate arrangement of flexible ester groups and rigid benzene rings in a molecular chain, so that the polycarbonate has wide application in the market. However, PC resins also suffer from poor processability, poor stress cracking resistance and poor solvent resistance, and impact properties are sensitive to notching, which also greatly limits their use. Polyethylene terephthalate (PET) as another engineering plastic has the advantages of excellent processing flowability, outstanding chemical resistance, low stress, low price and the like. However, it has disadvantages such as poor impact properties and long molding cycle. The advantages and the disadvantages of the two plastics are combined, and the PC/PET alloy material prepared by melt blending the two plastics can make up the respective defects. However, although both PC and PET belong to linear aromatic polyesters, the chemical results are similar, but the PC/PET alloy material obtained by blending the PC and PET belong to a typical amorphous/crystalline polymer system, the interface bonding strength is poor, and 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 various fields on the toughness of the alloy material. For this reason, toughening modification in a PC/PET alloy system is required. At present, a reactive compatibilizer or an elastomer is mainly adopted in a PC/PET alloy system for toughening, but the method can improve the impact resistance of the material and obviously reduce the strength and rigidity of the material. In addition, because ester group structures exist in molecular chains of PC and PET, ester exchange reaction is easy to occur in the high-temperature melt extrusion processing process, crystallization and melting behaviors of PET are influenced, and the PC/PET alloy material has extremely negative effects on the aspects of performance and molding stability of the PC/PET alloy material.
Disclosure of Invention
In order to overcome the defects of 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 has high strength and high impact resistance, and simultaneously has excellent thermal stability.
The method is realized by the following technical scheme:
a PC/PET alloy material comprises the following components in parts by weight:
further, the polycarbonate resin has a melt index of 3-20g/10min at 300 ℃/1.2kg as measured according to ISO 1133-1-2011 standard, and more preferably, the polycarbonate resin has a melt index of 8-15g/10min at 300 ℃/1.2 kg. 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 mold; if the melt index of the polycarbonate resin is too high, i.e., the viscosity is low, the heat-resistant stability of the material is poor, and the heat-resistant stability and the mechanical properties of the material are affected.
Further, the polyethylene terephthalate has a melt index of 10-35g/10min at 270 ℃/1.2kg as measured according to ISO 1133-1-2011 standards, and more preferably, the polyethylene terephthalate has a melt index of 19-25g/10min at 270 ℃/1.2 kg.
Further, the compound compatibilization 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, and 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 content of the ethylene-butyl acrylate-glycidyl methacrylate is low, the end capping effect on PET is poor, the risk of ester exchange reaction is increased, and the heat-resistant stability and the mechanical property of the final material are influenced. If the ratio of the ethylene-butyl acrylate-glycidyl methacrylate is too low, that is, 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 not good.
Further, the functionalized carbon nanotube is a carboxylated carbon nanotube, 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 toughening agent in the system is low, the functionalized carbon nano tube cannot play a good bridge role, and the effects of strengthening and toughening the functionalized carbon nano tube and improving the thermal stability of the functionalized carbon nano tube are influenced. Meanwhile, the end capping effect on PC and PET cannot be effectively realized, and the risk of side reaction is increased. The hydroxylation content is too high, the structure of the carbon nano tube is seriously damaged, and the performance of the carbon nano tube is influenced, so that the effects of strengthening and toughening the carbon nano tube and improving the thermal stability of the carbon nano tube are influenced.
The preparation method of the carboxylated carbon nanotube 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 for 1-2h at 80 ℃; then diluted with deionized water and left to settle for 24h until the supernatant was yellow. After removing the supernatant, the lower carbon nanotube dispersion liquid is filtered by a polyvinylidene fluoride microfiltration membrane with the aperture of 0.2 mu m, and is repeatedly washed by deionized water until the solution is neutral, and the carboxylated carbon nanotube is obtained after drying at the temperature of 100 ℃. 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 antioxidant or phosphite antioxidant, 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: carrying out melt extrusion and granulation on polyethylene terephthalate (PET) and functionalized carbon nanotubes by an extruder to prepare polyethylene terephthalate/carbon nanotube granules;
s3: and (3) premixing, melt extruding and granulating the polyethylene terephthalate/carbon nano tube granules, the polycarbonate, the compound compatibilizer and toughening agent and other processing aids prepared in the step (S2) to obtain the PC/PET alloy material.
Further, in steps S2 and S3, the melt extrusion process parameters 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 rotation speed of the screw 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, grids, spoilers and the like.
Compared with the prior art, the invention has the beneficial effects that:
1. through the optimized design of the formula, the PC matrix is a continuous phase within the weight parts of the PC and the PET respectively selected in the invention, so that the methyl methacrylate-butadiene-styrene copolymer in the compound compatibilization toughening agent can be selectively and uniformly dispersed in the PC continuous phase, thereby achieving a good toughening effect. In addition, the epoxy functional group of the ethylene-butyl acrylate-glycidyl methacrylate copolymer in the compound compatibilization toughening agent can chemically react with the end group of PET, so that the epoxy functional group is distributed at the phase interface of PC/PET, which is helpful for improving the interface compatibility between PC and PET, and has a synergistic effect with an ester exchange inhibitor, so that the degree of ester exchange reaction is reduced, the toughening effect is realized, and the melt processing stability is improved. And finally, adding the carboxylated carbon nano tube into the alloy system, and further reducing the generation of side reactions such as ester exchange and the like of the alloy material in the processes of high-temperature extrusion and subsequent injection molding processing by carrying out end capping on the carboxyl group of the carboxylated carbon nano tube and the end groups of PC and PET, thereby realizing the effect of high thermal stability.
2. According to the invention, through the optimized design of the process, PET is firstly melt-blended with the functionalized carbon nano-tubes and then is blended with PC, the compound compatibilizer and toughening agent and other auxiliaries, so that on one hand, the functionalized carbon nano-tubes can increase the melt viscosity of PET, thereby reducing the viscosity difference with PC resin and realizing the good dispersion of PET 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 of heterogeneous nucleation, so that the crystallization property of the PET material is reserved; meanwhile, a part of functionalized carbon nanotubes react with epoxy functional groups of the ethylene-butyl acrylate-glycidyl methacrylate copolymer in the compound compatibilization toughening agent, so that a bridge effect is achieved, the interface effect of PET and PC is further improved, and the effect of strengthening and toughening is realized.
3. The combination of formula and process cooperative optimization 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 technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
< production of examples and comparative examples >
The raw materials used in the examples and comparative examples of the present invention are commercially available, but are not limited to these materials:
polycarbonate resin a: melt index at 300 ℃/1.2kg of 10g/10min, brand PC 2100, available from Wanhua Shandong;
polycarbonate resin B: the melt index under the condition of 300 ℃/1.2kg is 20g/10min, the mark is PC 2220, and the melt index is purchased from Wanhua in Shandong province;
polycarbonate resin C: melt index at 300 deg.C/1.2 kg of 35g/10min, brand PC H-3000F, available from Mitsubishi, japan;
polycarbonate resin D: melt index at 300 ℃/1.2kg of 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 mark is PET BG80 which is purchased from China petrochemical characterization chemical fibers;
polyethylene terephthalate B: the melt index under the condition of 270 ℃/1.2kg is 35g/min, the mark is PET FG600, and the PET FG is purchased from petrochemical characterization chemical fibers;
methyl methacrylate-butadiene-styrene copolymer: number MBS EM500, available from LG chemistry;
ethylene-butyl acrylate-glycidyl methacrylate copolymer: no. AX8700, available from arkema, france;
functionalized carbon nanotube A: the carboxyl content is 1.5wt%, and the self-made product is prepared;
functionalized carbon nanotube B: the carboxyl content is 1wt%, and the self-made product is prepared;
functionalized carbon nanotube C: the carboxyl content is 2.5wt%, and the product is self-made;
functionalized carbon nanotube D: the carboxyl content is 0.6wt%, and the product is self-made;
functionalized carbon nanotube E: the carboxyl content is 2.8wt%, and the product is self-made;
carbon nanotube: the brand NTP3021, purchased from Nangang Limited, shenzhen;
ester exchange inhibitor: sodium dihydrogen phosphate, available from suzhou rich chemical technology ltd;
antioxidant A: tetrakis [ beta- (3,5-di-tert-butyl-4-hydroxyphenyl) propanoic acid ] pentaerythritol ester (i.e., antioxidant 1010), commercially available, in parallel, using the same commercial product;
and (3) antioxidant B: phosphite antioxidants, which are commercially available and are used in parallel experiments, are the same commercially available products;
lubricant: pentaerythritol stearate, commercially available, was used in parallel with the same commercial product.
The preparation methods of examples 1 to 15 of the present invention and comparative examples 1 to 8 are as follows:
s1, weighing the components according to the mixture ratio of the components shown in the tables 1, 2 and 5;
s2: carrying out melt blending and extrusion granulation on polyethylene terephthalate (PET) and a functionalized carbon nano tube by a double-screw extruder to prepare polyethylene terephthalate/carbon nano tube granules, wherein the melt 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: and (3) premixing, melt extruding and granulating the polyethylene terephthalate/carbon nano tube granules, the polycarbonate, the compound compatibilizer toughening agent 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 rotation speed of the screw was 400rpm.
Comparative example 9 was prepared as follows:
s1: weighing the components according to the formula of the example 1;
s2: premixing, melt extruding and granulating polyethylene terephthalate (PET), functionalized carbon nano tubes, polycarbonate, a compound compatibilization toughening agent and other processing aids to obtain the PC/PET alloy material. 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 rotational speed of the screw was 400rpm.
In the present specification, the term "part(s)" means "part(s) by weight" unless otherwise specified.
< test standards >
The performance test standards of the examples of the present invention and the comparative examples are as follows:
tensile strength: testing according to ISO 527-2-2012 standard, wherein the testing speed is 50mm/min;
flexural strength and flexural modulus: according to ISO 178-2019 standard, the testing speed is 2mm/min;
notched impact strength: according to ISO 179-1-2010 standard;
heat distortion temperature: adopting the method A according to ISO 75-2-2013 standard;
high thermal stability: and (3) respectively staying for 5min and 15min in the melt flow tester, testing the melt flow rate of the melt flow tester, and calculating the change rate of the melt index after respectively staying for 5min and 15 min. The smaller the change rate of the molten finger, the better the thermal stability of the alloy material.
TABLE 1 EXAMPLES 1-8 formulations
TABLE 2 EXAMPLES 9-15 formulations
TABLE 3 results of the Performance test of examples 1 to 8
TABLE 4 test results for examples 9-15
TABLE 5 comparative examples 1-9 formulations
TABLE 6 Performance test results for comparative examples 1-9
It can be seen from the above examples and comparative examples that the PC/PET alloy material prepared by adding the functionalized carbon nanotube, the methyl methacrylate-butadiene-styrene copolymer and the ethylene-butyl acrylate-glycidyl methacrylate copolymer for compounding and adopting the two-step preparation process has the characteristics of high strength, high impact resistance and high thermal stability, and is very suitable for automobile exterior parts such as bumpers, grilles, spoilers and the like.
Comparative example 1 compared to example 1, comparative example 1 did not have the addition of functionalized carbon nanotubes, resulting in comparative example 1 having low strength, poor impact resistance and poor thermal stability;
comparative examples 2, 3 in comparison with example 3, comparative example 2 did not add an ethylene-butyl acrylate-glycidyl methacrylate copolymer, and comparative example 3 did not add a methyl methacrylate-butadiene-styrene copolymer, i.e., both were not compounded using a methyl methacrylate-butadiene-styrene copolymer and an ethylene-butyl acrylate-glycidyl methacrylate copolymer, resulting in failure to achieve a balance in strength, impact resistance, and thermal stability of comparative examples 2, 3.
Comparative examples 4 and 5 have an out-of-range fraction of functionalized carbon nanotubes compared to example 1, resulting in deterioration of strength, flexural modulus, impact resistance and thermal stability of comparative examples 4 and 5.
Compared with the example 1, the addition amount of the compound compatibilization toughening agent in the comparative examples 6 and 7 exceeds the range, so that the strength, the flexural modulus, the impact resistance and the thermal stability of the comparative examples 6 and 7 are poor.
Comparative example 8 in comparison with example 1, comparative example 8 uses a common carbon nanotube, and comparative example 8 cannot achieve high strength, high impact resistance, and good thermal stability.
Comparative example 9 and example 1, both of which used the same formulation, were different in that comparative example 9 did not use the specific preparation method provided by the present invention, resulting in poor performance of comparative example 9.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The PC/PET alloy material is characterized by comprising the following components in parts by weight:
the compound compatibilization toughening agent is a methyl methacrylate-butadiene-styrene copolymer and an ethylene-butyl acrylate-glycidyl methacrylate copolymer.
2. The PC/PET alloy material according to 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 according to claim 1, wherein the melt index of the polyethylene terephthalate at 270 ℃/1.2kg is 10-35g/min.
4. The PC/PET alloy material according to claim 1, wherein the weight ratio of the methyl methacrylate-butadiene-styrene copolymer to the ethylene-butyl acrylate-glycidyl methacrylate copolymer is 1:1-3:1.
5. The PC/PET alloy material of claim 1, wherein the functionalized carbon nanotubes are carboxylated carbon nanotubes.
6. The PC/PET alloy material as claimed in claim 5, wherein the carboxylated carbon nanotubes have a carboxyl group content of 1-2.5wt%.
7. The PC/PET alloy material of claim 1, wherein the transesterification inhibitor is sodium dihydrogen phosphate.
8. The PC/PET alloy material according to claim 1, wherein the other processing aid is at least one of an antioxidant and a lubricant.
9. A method for preparing the PC/PET alloy material according to any one of claims 1 to 8, comprising the steps of:
s1: weighing the components according to the proportion;
s2: carrying out melt extrusion and granulation on polyethylene terephthalate and the functionalized carbon nano tube by an extruder to prepare polyethylene terephthalate/carbon nano tube granules;
s3: and (3) premixing, melt extruding and granulating the polyethylene terephthalate/carbon nano tube granules, the polycarbonate, the compound compatibilizer and toughening agent and other processing aids prepared in the step (S2) to obtain the PC/PET alloy material.
10. Use of the PC/PET alloy material according to any one of claims 1 to 8 for the production of automotive exterior parts.
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