CN113789040B - High-rigidity high-modulus antistatic PC composition and preparation method thereof - Google Patents
High-rigidity high-modulus antistatic PC composition and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
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Abstract
The invention relates to the technical field of polycarbonate, in particular to a high-rigidity high-modulus antistatic PC composition and a preparation method thereof, wherein the PC composition comprises the following raw materials: 70-80 parts of PC, 15-25 parts of glass fiber, 20-30 parts of polyketone/PA blend, 10-12 parts of antistatic agent, 4-6 parts of toughening agent, 1-3 parts of compatilizer, 0.2-0.4 part of antioxidant and 0.3-0.5 part of lubricant. The invention is a blending modification system which takes polycarbonate as a continuous phase and adds polyketone, PA66, glass fiber, antistatic agent and the like as a disperse phase, and has the performances of high strength, high modulus, antistatic property, chemical resistance and the like.
Description
Technical Field
The invention relates to the technical field of polycarbonate, in particular to a high-rigidity high-modulus antistatic PC composition and a preparation method thereof.
Background
Polycarbonate (abbreviated as PC in english) 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, depending on the structure of the ester groups. Among them, aliphatic and aliphatic-aromatic polycarbonates have limited their use as engineering plastics due to their low mechanical properties. Aromatic polycarbonates are the predominant plastics in development for general use. Polycarbonate has very good performances such as impact strength, elastic modulus, dimensional stability and the like, but is easy to generate stress cracking, high in notch impact sensitivity and the like, and is also a defect of polycarbonate, and a toughening agent is still required to be added for modification generally. But the addition of the toughening agent inevitably causes the reduction of the rigidity performances such as the tensile strength, the bending strength and the like of the polycarbonate. In addition, polycarbonates have a general problem with respect to their chemical resistance.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a PC composition with high rigidity, high modulus, static resistance and chemical resistance and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
the high-rigidity high-modulus antistatic PC composition comprises the following raw materials in parts by weight:
the preparation method of the polyketone/PA blend comprises the following steps: adding 10-15 parts by weight of polyketone, 10-15 parts by weight of PA66 and 150-200 parts by weight of solvent into a reaction kettle, heating to 160-170 ℃ in the atmosphere of high-pressure inert gas, preserving heat for 1-3h, then cooling to room temperature at the cooling rate of 1-3 ℃/min under the stirring condition, and finally carrying out solid-liquid separation, drying and sieving to obtain the polyketone/PA blend.
Polyketone is a novel green polymer material synthesized by carbon monoxide and olefin, has the properties of excellent permeability resistance, high barrier property, high tensile strength, high impact strength, high elongation at break and the like, can obviously improve the mechanical property and chemical resistance when added into polycarbonate, has the characteristic of high rigidity and high modulus when added into the polycarbonate, and can also improve the rigidity strength and the notch impact strength when added into the polycarbonate. Therefore, the invention uses polycarbonate as a continuous phase, and polyketone, PA66, glass fiber, antistatic agent and the like are added as a blending modification system of a dispersed phase, so as to obtain the properties of high strength, high modulus, static resistance and chemical resistance. However, the invention has a plurality of different dispersed phases, which easily causes the problem of serious phase separation degree, and the PA66 serves as a rigid body in PC for toughening, under the condition that glass fiber, antistatic agent and toughening agent exist, the toughening effect of the PA66 is not obvious, and the reinforcing effect is not as obvious as that of the glass fiber. Therefore, the PA66 is not only used for simple physical property superposition, but also used for better improving various performances of the PC composition by a method of solvent dissolution, precipitation and regeneration, wherein the precipitated small-particle PA66 is attached to the surface of large-particle polyketone to form a blend body with a core-shell structure, the PA66 serving as a rigid body can initiate stress concentration to more efficiently transmit impact energy to the polyketone of a core, and the impact energy is consumed between the polyketone/PA blend body and the PC by generating defects such as silver streaks, cavities and the like, so that the notch impact strength of the PC composition is remarkably improved, meanwhile, the PA66 and the polyketone have certain compatibility, the polyketone/PA blend body formed by the two components is less prone to phase separation, and the degree of phase separation of the polycarbonate composition is equivalently reduced.
Wherein the solvent consists of ethanol and n-butanol according to the weight ratio of 80-90. The alcohol solvent has low toxicity, the boiling point of the ethanol/n-butanol mixed solvent can be increased by pressurizing, so that the PA66 can be dissolved under the high-temperature condition, and the polyketone has good chemical resistance, so that the polyketone can keep a solid state in the solvent.
Wherein the polyketone is POK M330A.
Wherein the glass fiber is alkali-free glass fiber with the diameter of 10-20 μm.
Wherein the antistatic agent is at least one of conductive carbon black, carbon nanotubes and graphene. Preferably, the antistatic agent is conductive carbon black, and the cost is low.
Wherein the toughening agent consists of S-2001 and 1125AC in a weight ratio of 3-5:1. S-2001 and 1125AC are both low temperature tougheners, which can better improve the impact strength of the PC composition at low temperature.
The compatilizer is POE-g-MAH, which is beneficial to improving the interfacial bonding energy of the PC and the polyketone/PA blend, and simultaneously, due to the existence of an active group MAH, the glass fiber and the PC resin have better compatibility, so that the floating fiber can be reduced.
Wherein the antioxidant consists of an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:1-3.
Wherein, the lubricant is a high-temperature bright lubricant PETS.
The preparation method of the antistatic PC composition with high rigidity and high modulus comprises the following steps: mixing PC, polyketone/PA blend, antistatic agent, toughening agent, compatilizer, antioxidant and lubricant, feeding into a main feeding port of a double-screw extruder, feeding glass fiber from a side feeding port of the double-screw extruder, and performing melt extrusion granulation to obtain the high-rigidity high-modulus antistatic PC composition.
The invention has the beneficial effects that:
1. the invention takes polycarbonate as a continuous phase, and adds polyketone, PA66, glass fiber, antistatic agent and the like as a blending modification system of a disperse phase, and the invention has the performances of high strength, high modulus, antistatic property, chemical resistance and the like;
2. according to the invention, by a solvent dissolution precipitation regeneration method, the precipitated small-particle PA66 is attached to the surface of large-particle polyketone to form a blended body with a core-shell structure, the PA66 serving as a rigid body can initiate stress concentration and more efficiently transmit impact energy to the polyketone of a core, and the impact energy is consumed between the polyketone/PA blended body and a PC through generating defects such as silver streaks, cavities and the like, so that the notch impact strength of the PC composition is remarkably improved, meanwhile, the PA66 and the polyketone have certain compatibility, the polyketone/PA blended body formed by the PA66 and the polyketone is less prone to phase separation, which is equivalent to the reduction of the phase separation degree of the polycarbonate composition, thereby better improving various performances of the PC composition;
3. the bubble glacial acetic acid is not cracked within 10 minutes, and the time for conventionally testing the bubble glacial acetic acid by using the PC + GF material which is usually used for the middle frame of the smart phone is only 5 minutes.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
The high-rigidity high-modulus antistatic PC composition comprises the following raw materials in parts by weight:
the preparation method of the polyketone/PA blend comprises the following steps: adding 12.5 parts by weight of polyketone, 12.5 parts by weight of PA66 and 175 parts by weight of solvent into a reaction kettle, heating to 165 ℃ in the atmosphere of high-pressure inert gas, preserving heat for 2 hours, then cooling to room temperature at a cooling rate of 2 ℃/min under the stirring condition, and finally carrying out solid-liquid separation, drying and sieving to obtain the polyketone/PA blend.
Wherein the solvent consists of ethanol and n-butanol according to the weight ratio of 85.
Wherein the polyketone is POK M330A.
Wherein the glass fiber is alkali-free glass fiber with the diameter of 14 μm and the model of EDR14-2000-988A.
Wherein the antistatic agent is conductive carbon black.
Wherein the toughening agent consists of S-2001 and 1125AC in a weight ratio of 4:1.
Wherein, the compatilizer is POE-g-MAH.
Wherein the antioxidant consists of an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
Wherein, the lubricant is a high-temperature bright lubricant PETS.
The preparation method of the antistatic PC composition with high rigidity and high modulus comprises the following steps: mixing PC, polyketone/PA blend, antistatic agent, toughening agent, compatilizer, antioxidant and lubricant, feeding into a main feeding port of a double-screw extruder, feeding glass fiber from a side feeding port of the double-screw extruder, and performing melt extrusion granulation to obtain the high-rigidity high-modulus antistatic PC composition.
Example 2
The high-rigidity high-modulus antistatic PC composition comprises the following raw materials in parts by weight:
the preparation method of the polyketone/PA blend comprises the following steps: adding 15 parts by weight of polyketone, 15 parts by weight of PA66 and 200 parts by weight of solvent into a reaction kettle, heating to 170 ℃ in the atmosphere of high-pressure inert gas, preserving heat for 1h, then cooling to room temperature at a cooling rate of 3 ℃/min under the stirring condition, and finally carrying out solid-liquid separation, drying and sieving to obtain the polyketone/PA blend.
Wherein the solvent consists of ethanol and n-butanol according to a weight ratio of 90.
Wherein the polyketone is POK M330A.
Wherein the glass fiber is alkali-free glass fiber with the diameter of 20 μm.
Wherein the antistatic agent is carbon nanotubes.
Wherein the toughening agent consists of S-2001 and 1125AC in a weight ratio of 5:1.
Wherein, the compatilizer is POE-g-MAH.
Wherein the antioxidant consists of an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:3.
Wherein, the lubricant is a high-temperature bright lubricant PETS.
The preparation method of the antistatic PC composition with high rigidity and high modulus comprises the following steps: mixing PC, polyketone/PA blend, antistatic agent, toughening agent, compatilizer, antioxidant and lubricant, feeding into a main feeding port of a double-screw extruder, feeding glass fiber from a side feeding port of the double-screw extruder, and performing melt extrusion granulation to obtain the high-rigidity high-modulus antistatic PC composition.
Example 3
The high-rigidity high-modulus antistatic PC composition comprises the following raw materials in parts by weight:
the preparation method of the polyketone/PA blend comprises the following steps: adding 10 parts by weight of polyketone, 10 parts by weight of PA66 and 150 parts by weight of solvent into a reaction kettle, heating to 160 ℃ in the atmosphere of high-pressure inert gas, preserving heat for 3 hours, then cooling to room temperature at a cooling rate of 1 ℃/min under the stirring condition, and finally carrying out solid-liquid separation, drying and sieving to obtain the polyketone/PA blend.
Wherein the solvent consists of ethanol and n-butanol according to a weight ratio of 80.
Wherein the polyketone is POK M330A.
Wherein the glass fiber is alkali-free glass fiber with the diameter of 10 μm.
Wherein, the antistatic agent is graphene.
Wherein the toughening agent consists of S-2001 and 1125AC in a weight ratio of 3:1.
Wherein, the compatilizer is POE-g-MAH.
Wherein the antioxidant consists of an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:1.
Wherein, the lubricant is a high-temperature bright lubricant PETS.
The preparation method of the antistatic PC composition with high rigidity and high modulus comprises the following steps: mixing PC, a polyketone/PA blend, an antistatic agent, a toughening agent, a compatilizer, an antioxidant and a lubricant, then feeding the mixture into a main feeding port of a double-screw extruder, feeding glass fibers into the main feeding port of the double-screw extruder from a side feeding port of the double-screw extruder, and performing melt extrusion granulation to obtain the high-rigidity high-modulus antistatic PC composition.
Comparative example 1
A PC composition comprises the following raw materials in parts by weight:
the preparation method of the regenerated PA66 comprises the following steps: adding 12.5 parts by weight of PA66 and 150 parts by weight of solvent into a reaction kettle, heating to 165 ℃ in the atmosphere of high-pressure inert gas, preserving the temperature for 2 hours, then cooling to room temperature at a cooling rate of 2 ℃/min under the stirring condition, and finally carrying out solid-liquid separation, drying and sieving to obtain the regenerated PA66.
Wherein the solvent consists of ethanol and n-butanol according to the weight ratio of 85.
Wherein the polyketone is POK M330A.
Wherein the glass fiber is alkali-free glass fiber, has a diameter of 14 μm and is EDR14-2000-988A.
Wherein the antistatic agent is conductive carbon black.
Wherein the toughening agent consists of S-2001 and 1125AC in a weight ratio of 4:1.
Wherein, the compatilizer is POE-g-MAH.
Wherein the antioxidant consists of an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
Wherein, the lubricant is a high-temperature bright lubricant PETS.
A method of making a PC composition as described above: stirring and dispersing polyketone and regenerated PA66 in sufficient water, filtering, washing and drying, mixing with PC, an antistatic agent, a toughening agent, a compatilizer, an antioxidant and a lubricant, feeding into a main feeding port of a double-screw extruder, feeding glass fiber from a side feeding port of the double-screw extruder, and performing melt extrusion granulation to obtain the PC composition.
Comparative example 2
A PC composition comprises the following raw materials in parts by weight:
wherein the solvent consists of ethanol and n-butanol according to the weight ratio of 85.
Wherein the polyketone is POK M330A.
Wherein the glass fiber is alkali-free glass fiber with the diameter of 14 μm and the model of EDR14-2000-988A.
Wherein the antistatic agent is conductive carbon black.
Wherein the toughening agent consists of S-2001 and 1125AC in a weight ratio of 4:1.
Wherein, the compatilizer is POE-g-MAH.
Wherein the antioxidant consists of an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
Wherein, the lubricant is a high-temperature bright lubricant PETS.
A method of making a PC composition as described above: mixing PC, polyketone, an antistatic agent, a toughening agent, a compatilizer, an antioxidant and a lubricant, then adding the mixture into a main feeding port of a double-screw extruder, adding glass fiber from a side feeding port of the double-screw extruder, and carrying out melt extrusion granulation to obtain the PC composition.
The PC compositions of example 1 and comparative examples 1-2 were subjected to mechanical property tests, the test items and standards being as follows:
tensile strength: GB/T1040.2-2006
Flexural strength and flexural modulus: GB/T9341-2008
Impact strength of the simply supported beam notch: GB/T1043.1-2008
In comparative example 2, the polycarbonate is modified by polyketone and glass fiber, so that the polycarbonate has better tensile strength, bending modulus and notch impact strength, in comparative example 1, PA66 is added for modification, the consumption of the polyketone is reduced, PA66 is not as good as the polyketone in toughness, and although the polycarbonate has better tensile strength, the mechanical property is reduced, particularly the rigidity is reduced, due to the phase separation caused by introducing more dispersed phases, so that the overall mechanical property is not as good as that of directly modifying the polyketone, and in example 1 of the invention, the dispersion state of PA66 and the polyketone is improved by solvent precipitation regeneration, the phase separation degree is reduced, the toughening effect of the polyketone is strengthened, and the best mechanical property is achieved.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit and scope of the present invention.
Claims (9)
1. A high rigidity high modulus antistatic PC composition, characterized in that: the feed comprises the following raw materials in parts by weight:
70-80 parts of PC
15-25 parts of glass fiber
20-30 parts of polyketone/PA blend
10-12 parts of antistatic agent
4-6 parts of toughening agent
1-3 parts of compatilizer
0.2 to 0.4 portion of antioxidant
0.3-0.5 part of a lubricant;
the preparation method of the polyketone/PA blend comprises the following steps: adding 10-15 parts by weight of polyketone, 10-15 parts by weight of PA66 and 150-200 parts by weight of solvent into a reaction kettle, heating to 160-170 ℃ in the atmosphere of high-pressure inert gas, preserving heat for 1-3h, then cooling to room temperature at the cooling rate of 1-3 ℃/min under the stirring condition, and finally carrying out solid-liquid separation, drying and sieving to obtain the polyketone/PA blend;
the solvent consists of ethanol and n-butanol according to the weight ratio of 80-90.
2. The high rigidity and high modulus antistatic PC composition according to claim 1, characterized in that: the polyketone is POK M330A.
3. The high rigidity and high modulus antistatic PC composition according to claim 1, characterized in that: the glass fiber is alkali-free glass fiber with the diameter of 10-20 μm.
4. The high rigidity and high modulus antistatic PC composition according to claim 1, characterized in that: the antistatic agent is at least one of conductive carbon black, carbon nano tubes and graphene.
5. The high rigidity and high modulus antistatic PC composition according to claim 1, characterized in that: the toughening agent consists of S-2001 and 1125AC in a weight ratio of 3-5:1.
6. The high rigidity and high modulus antistatic PC composition according to claim 1, characterized in that: the compatilizer is POE-g-MAH.
7. The high rigidity and high modulus antistatic PC composition according to claim 1, characterized in that: the antioxidant consists of an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:1-3.
8. The high rigidity high modulus antistatic PC composition according to claim 1, characterized in that: the lubricant is high-temperature-resistant bright lubricant PETS.
9. The method for preparing a high rigidity high modulus antistatic PC composition according to any one of claims 1 to 8, wherein: mixing PC, a polyketone/PA blend, an antistatic agent, a toughening agent, a compatilizer, an antioxidant and a lubricant, then adding the mixture into a main feeding port of a double-screw extruder, adding glass fiber from a side feeding port of the double-screw extruder, and carrying out melt extrusion granulation to obtain the high-rigidity high-modulus antistatic PC composition.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197082A (en) * | 1997-03-05 | 1998-10-28 | 希尔斯股份公司 | Preparation of precipitated polymide powders of narrow particle size distribution and low porosity |
| CN109401302A (en) * | 2018-10-26 | 2019-03-01 | 广东圆融新材料有限公司 | Good surface high impact nylon/POK alloy and preparation method thereof |
| WO2020212662A1 (en) * | 2019-04-19 | 2020-10-22 | Arkema France | Particles of polyamide powders and use thereof in powder agglomeration processes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| DE102011078721A1 (en) * | 2011-07-06 | 2013-01-10 | Evonik Degussa Gmbh | Powder containing polymer-coated polymeric core particles |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197082A (en) * | 1997-03-05 | 1998-10-28 | 希尔斯股份公司 | Preparation of precipitated polymide powders of narrow particle size distribution and low porosity |
| CN109401302A (en) * | 2018-10-26 | 2019-03-01 | 广东圆融新材料有限公司 | Good surface high impact nylon/POK alloy and preparation method thereof |
| WO2020212662A1 (en) * | 2019-04-19 | 2020-10-22 | Arkema France | Particles of polyamide powders and use thereof in powder agglomeration processes |
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