CN111253746A - Electrical insulation thermoplastic resin composition and preparation method and application thereof - Google Patents
Electrical insulation thermoplastic resin composition and preparation method and application thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
- C08L81/02—Polythioethers; Polythioether-ethers
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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
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Abstract
The invention provides an electrical insulation thermoplastic resin composition, a preparation method and an application thereof, wherein the electrical insulation thermoplastic resin composition comprises the following raw materials in parts by weight: 40-70 parts of polyimide; 10-40 parts of polyphenylene sulfide; 15-40 parts of silicon powder and 0.45-1.2 parts of coupling agent. The electrical insulation thermoplastic resin composition provided by the invention adopts polyimide, polyphenylene sulfide, silicon micropowder and coupling agent as raw materials, and the dosage of each raw material is limited, so that the electrical insulation thermoplastic resin composition has excellent mechanical property, electrical insulation property, flame retardant property and heat resistance, low thermal expansion coefficient and excellent comprehensive performance, can meet the application under complex working conditions of large capacity, high field strength, high mechanical load, high temperature field and the like, and can be recycled.
Description
Technical Field
The invention relates to the technical field of electrical insulation materials, in particular to an electrical insulation thermoplastic resin composition and a preparation method and application thereof.
Background
The electrical insulating material is a key material for manufacturing electrical equipment and is also an important component of high-voltage electrical equipment. With the development of the electric power industry in China to the aspects of large capacity, high field strength, high mechanical load, high temperature field and the like, higher and higher requirements on the quality and reliability of the electric insulating material are provided.
At present, thermosetting plastic epoxy resin is widely applied to high-voltage insulation equipment due to excellent mechanical property and insulation property, but the mechanical property and the insulation property of the epoxy resin are obviously reduced under high-temperature conditions, and unrecoverable thermoelectric aging and discharge ablation damage exist, so that the epoxy resin cannot meet the application under complex working conditions of high capacity, high field strength, high mechanical load, high temperature field and the like.
And the current other electrical insulation materials can not satisfy the application under the complicated operating mode condition yet, if: chinese patent document CN104817831A discloses an electrical insulation thermoplastic resin composition, which is prepared from thermoplastic resin, reinforcing filler, compatibilizer, plasticizer and coupling agent as raw materials, wherein the thermoplastic resin is at least one of polyamide, polyphenylene sulfide, polybutylene terephthalate and polycarbonate, and the coupling agent is a silane coupling agent or titanate coupling agent; the electrically insulating thermoplastic resin composition disclosed in this document has poor heat resistance and flame retardancy, although it has excellent electrical insulating properties and high compressive strength.
The thermoplastic resin composite material disclosed in chinese patent document CN105907095A comprises polyphenylene sulfide, nylon 66, chopped alkali-free glass fiber, nano-montmorillonite, compatibilizer, toughening agent, coupling agent, antioxidant and heat stabilizer; the polyphenylene sulfide is linear polyphenylene sulfide, and the coupling agent is at least one of silane coupling agent KH-550 and titanate coupling agent. The thermoplastic resin composite disclosed in this document has good mechanical properties and processability, but has insufficient heat resistance and poor electrical insulation properties.
Therefore, the electrical insulating material which has excellent comprehensive performance and can meet the application requirements under complex working conditions such as high capacity, high field strength, high mechanical load and high temperature field has important significance for the development of the power industry.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects that the electrical insulating material in the prior art has poor comprehensive performance and cannot meet the application under complex working conditions such as high capacity, high field strength, high mechanical load, high temperature field and the like, thereby providing the electrical insulating thermoplastic resin composition, and the preparation method and the application thereof.
Therefore, the invention provides the following technical scheme:
an electrical insulation thermoplastic resin composition comprises the following raw materials in parts by weight: 40-70 parts of polyimide; 10-40 parts of polyphenylene sulfide; 15-40 parts of silicon powder and 0.45-1.2 parts of coupling agent.
The polyimide is a thermoplastic polyimide.
The polyphenylene sulfide is linear polyphenylene sulfide.
The silicon micro powder is fused silicon micro powder;
the median particle diameter D50 of the silicon micropowder is 5-30 um.
The coupling agent is at least one of silane coupling agents KH550, KH560, KH570, KH580 and KH 602.
The mass ratio of the polyimide to the polyphenylene sulfide is 1.8-4.0: 1.
The present invention also provides a method for preparing the above-mentioned electrical insulation thermoplastic resin composition, comprising the steps of:
activating the silicon micropowder by using a coupling agent;
and uniformly mixing the activated coupling agent, polyimide and polyphenylene sulfide, and then extruding, granulating and drying to obtain the electrical insulation thermoplastic resin composition.
The step of activating the silicon micropowder by using the coupling agent is to uniformly mix the coupling agent and the silicon micropowder and dry the mixture.
The extrusion granulation adopts a double-screw extruder, and the technological parameters of the double-screw extruder comprise: the temperature of the feeding section is 340-.
The invention also provides the application of the electrical insulation thermoplastic resin composition or the electrical insulation thermoplastic resin composition prepared by the preparation method of the electrical insulation thermoplastic resin composition in high-voltage insulation parts or high-power chip plastic package.
The technical scheme of the invention has the following advantages:
1. according to the electrical insulation thermoplastic resin composition provided by the invention, polyimide, polyphenylene sulfide, silicon micropowder and coupling agent are used as raw materials, and the dosage of each raw material is limited, so that the electrical insulation thermoplastic resin composition has excellent mechanical property, electrical insulation property, flame retardant property and heat resistance, is low in thermal expansion coefficient and excellent in comprehensive performance, can meet the application under complex working conditions of large capacity, high field strength, high mechanical load, high temperature field and the like, and can be recycled.
2. The electric insulation thermoplastic resin composition provided by the invention can effectively reduce the processing temperature by adopting the thermoplastic polyimide and the linear polyphenylene sulfide, is easy to process and form, and has high consistency.
3. The electrical insulation thermoplastic resin composition provided by the invention can effectively improve and reduce the thermal expansion coefficient of the composition and improve the mechanical strength by limiting the median particle size of the silicon micropowder; if the median particle size of the silicon micropowder is too small, the viscosity of the system is high, and the silicon micropowder is difficult to process; too large a median particle diameter results in poor homogeneity and low mechanical strength of the composition.
4. The electrical insulation thermoplastic resin composition provided by the invention can further improve the comprehensive performance of products by limiting the mass ratio of the polyimide to the polyphenylene sulfide.
5. According to the preparation method of the electrical insulation thermoplastic resin composition, the silicon micropowder is activated by using the coupling agent, so that the interface compatibility of the silicon micropowder, polyimide and polyphenylene sulfide can be improved; then the electric insulation thermoplastic resin composition obtained by melting, blending, extruding, granulating and drying has excellent mechanical property, electric insulation property, flame retardant property and heat resistance, low thermal expansion coefficient and excellent comprehensive performance, can meet the application under complex working conditions of large capacity, high field strength, high mechanical load, high temperature field and the like, and can be recycled.
6. The electrical insulation thermoplastic resin composition provided by the invention has high stability and life cycle in high-voltage insulation parts or high-power chip plastic package.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
Example 1
This example provides an electrically insulating thermoplastic resin composition, which is prepared by a process comprising the steps of:
activation of the silicon micropowder: mixing 15kg of fused silica micropowder (with median particle diameter D50 of 20um) and 1.0kg of coupling agent KH550 at 100 deg.C in a high-speed disperser for 30min, taking out, and drying in a forced air oven at 120 deg.C for 5 h;
respectively drying thermoplastic polyimide and linear polyphenylene sulfide in a blast oven at 150 ℃ for 5 hours for later use;
weighing 60kg of dried thermoplastic polyimide and 24kg of dried linear polyphenylene sulfide, adding the weighed dried thermoplastic polyimide and the activated silicon micro powder into a high-speed batching mixer, and uniformly mixing to obtain a premix;
adding the premix into a double-screw extruder, extruding and granulating, and drying the obtained granules to obtain the electrical insulation thermoplastic resin composition; wherein the temperature of a feeding section in the double-screw extruder is 350 ℃, the temperature of a plasticizing shearing section is 365 ℃, the temperature of a machine head is 375 ℃, the rotating speed of a screw is 70r/min, and the rotating speed of grain cutting is 150 r/min.
Example 2
This example provides an electrically insulating thermoplastic resin composition, which is prepared by a process comprising the steps of:
activation of the silicon micropowder: mixing 40kg of fused silica micropowder (with median particle diameter D50 of 5um) and 1.2kg of coupling agent KH550 at 120 deg.C in a high-speed disperser for 30min, taking out, and drying in a forced air oven at 150 deg.C for 3 h;
respectively drying thermoplastic polyimide and linear polyphenylene sulfide in a blast oven for 8 hours at 120 ℃ for later use;
weighing 40kg of dried thermoplastic polyimide and 10kg of dried linear polyphenylene sulfide, adding the weighed dried thermoplastic polyimide and the activated silicon micro powder into a high-speed batching mixer, and uniformly mixing to obtain a premix;
adding the premix into a double-screw extruder, extruding and granulating, and drying the obtained granules to obtain the electrical insulation thermoplastic resin composition; wherein the temperature of the feeding section in the double-screw extruder is 340 ℃, the temperature of the plasticizing shearing section is 380 ℃, the temperature of the machine head is 380 ℃, the rotating speed of the screw is 65r/min, and the rotating speed of the grain cutting is 110 r/min.
Example 3
This example provides an electrically insulating thermoplastic resin composition, which is prepared by a process comprising the steps of:
activation of the silicon micropowder: mixing 35kg of fused silica micropowder (with a median particle diameter D50 of 30um), 0.45kg of coupling agent KH560 and 0.4kg of coupling agent KH602 in a high-speed dispersion machine at 110 ℃ for 30min, taking out, and drying in a blast oven at 130 ℃ for 4h for later use;
respectively drying thermoplastic polyimide and linear polyphenylene sulfide in a blast oven at 140 ℃ for 6 hours for later use;
weighing 54kg of dried thermoplastic polyimide and 30kg of dried linear polyphenylene sulfide, adding the weighed dried thermoplastic polyimide and the activated silicon micropowder into a high-speed batching mixer, and uniformly mixing to obtain a premix;
adding the premix into a double-screw extruder, extruding and granulating, and drying the obtained granules to obtain the electrical insulation thermoplastic resin composition; wherein the temperature of a feeding section in the double-screw extruder is 360 ℃, the temperature of a plasticizing shearing section is 375 ℃, the temperature of a machine head is 370 ℃, the rotating speed of a screw is 100r/min, and the rotating speed of grain cutting is 120 r/min.
Example 4
This example provides an electrically insulating thermoplastic resin composition, which is prepared by a process comprising the steps of:
activation of the silicon micropowder: mixing 20kg of fused silica micropowder (with median particle diameter D50 of 15um) and 0.45kg of coupling agent KH580 in a high-speed dispersion machine at 100 ℃ for 30min, taking out, and drying in a forced air oven at 120 ℃ for 5h for later use;
respectively drying thermoplastic polyimide and linear polyphenylene sulfide in a blast oven at 160 ℃ for 5 hours for later use;
weighing 70kg of dried thermoplastic polyimide and 40kg of dried linear polyphenylene sulfide, adding the dried thermoplastic polyimide and the activated silicon micropowder into a high-speed batching mixer, and uniformly mixing to obtain a premix;
adding the premix into a double-screw extruder, extruding and granulating, and drying the obtained granules to obtain the electrical insulation thermoplastic resin composition; wherein the temperature of the feeding section in the double-screw extruder is 345 ℃, the temperature of the plasticizing shearing section is 370 ℃, the temperature of the machine head is 375 ℃, the rotating speed of the screw is 90r/min, and the rotating speed of the grain cutting is 140 r/min.
Example 5
This example provides an electrically insulating thermoplastic resin composition, which is prepared by a process comprising the steps of:
activation of the silicon micropowder: mixing 30kg of fused silica micropowder (with median particle diameter D50 of 25um) and 0.6kg of coupling agent KH570 at 105 deg.C in a high-speed disperser for 30min, taking out, and drying in a forced air oven at 125 deg.C for 4 h;
respectively drying thermoplastic polyimide and linear polyphenylene sulfide in a blast oven at 180 ℃ for 3h for later use;
weighing 40kg of dried thermoplastic polyimide and 40kg of dried linear polyphenylene sulfide, adding the weighed dried thermoplastic polyimide and the dried linear polyphenylene sulfide into a high-speed batching mixer, and uniformly mixing to obtain a premix;
adding the premix into a double-screw extruder, extruding and granulating, and drying the obtained granules to obtain the electrical insulation thermoplastic resin composition; wherein the temperature of the feeding section in the double-screw extruder is 355 ℃, the temperature of the plasticizing shearing section is 365 ℃, the temperature of the machine head is 380 ℃, the rotating speed of the screw is 80r/min, and the rotating speed of the grain cutting is 160 r/min.
Example 6
This example provides an electrically insulating thermoplastic resin composition, which is prepared by a process comprising the steps of:
activation of the silicon micropowder: mixing 25kg of fused silica micropowder (with a median particle diameter D50 of 20um), 0.35kg of coupling agent KH570, 0.3kg of coupling agent KH580 and 0.3kg of coupling agent KH560 in a high-speed dispersion machine at 100 ℃ for 30min, taking out, and drying in an air-blast oven at 120 ℃ for 5h for later use;
respectively drying thermoplastic polyimide and linear polyphenylene sulfide in a blast oven at 150 ℃ for 5 hours for later use;
weighing 70kg of dried thermoplastic polyimide and 10kg of dried linear polyphenylene sulfide, adding the dried thermoplastic polyimide and the activated silicon micro powder into a high-speed batching mixer, and uniformly mixing to obtain a premix;
adding the premix into a double-screw extruder, extruding and granulating, and drying the obtained granules to obtain the electrical insulation thermoplastic resin composition; wherein the temperature of the feeding section in the double-screw extruder is 350 ℃, the temperature of the plasticizing shearing section is 380 ℃, the temperature of the machine head is 370 ℃, the rotating speed of the screw is 95r/min, and the rotating speed of the grain cutting is 105 r/min.
Comparative example 1
The present comparative example provides an electrical insulating thermoplastic resin composition, the preparation method of which comprises the steps of:
activation of the silicon micropowder: mixing 15kg of fused silica micropowder (with median particle diameter D50 of 20um) and 1.0kg of coupling agent KH550 at 100 deg.C in a high-speed disperser for 30min, taking out, and drying in a forced air oven at 120 deg.C for 5 h;
respectively drying linear polyphenylene sulfide in a blast oven at 150 ℃ for 5h for later use;
weighing 24kg of dried linear polyphenylene sulfide, adding the weighed linear polyphenylene sulfide and the activated silicon micropowder into a high-speed batching mixer, and uniformly mixing to obtain a premix;
adding the premix into a double-screw extruder, extruding and granulating, and drying the obtained granules to obtain the electrical insulation thermoplastic resin composition; wherein the temperature of the feeding section in the double-screw extruder is 270 ℃, the temperature of the plasticizing shearing section is 275 ℃, the temperature of a machine head is 285 ℃, the rotating speed of the screw is 70r/min, and the rotating speed of the grain cutting is 150 r/min.
Comparative example 2
The present comparative example provides an electrical insulating thermoplastic resin composition, the preparation method of which comprises the steps of:
respectively drying thermoplastic polyimide and linear polyphenylene sulfide in a blast oven at 150 ℃ for 5 hours for later use;
weighing 1.0kg of coupling agent (KH550), 60kg of dried thermoplastic polyimide and 24kg of dried linear polyphenylene sulfide; then adding the mixture into a high-speed batching mixer, and uniformly mixing to obtain a premix;
adding the premix into a double-screw extruder, extruding and granulating, and drying the obtained granules to obtain the electrical insulation thermoplastic resin composition; wherein the temperature of a feeding section in the double-screw extruder is 350 ℃, the temperature of a plasticizing shearing section is 365 ℃, the temperature of a machine head is 375 ℃, the rotating speed of a screw is 70r/min, and the rotating speed of grain cutting is 150 r/min.
Comparative example 3
The present comparative example provides an electrical insulating thermoplastic resin composition, the preparation method of which comprises the steps of:
respectively drying thermoplastic polyimide and linear polyphenylene sulfide in a blast oven at 150 ℃ for 5 hours for later use;
weighing 60kg of dried thermoplastic polyimide, 24kg of dried linear polyphenylene sulfide, 15kg of fused silica micropowder (the median particle size D50 is 20um) and 1.0kg of coupling agent KH550, adding the fused silica micropowder and the coupling agent KH550 into a high-speed batching mixer, and uniformly mixing to obtain a premix;
adding the premix into a double-screw extruder, extruding and granulating, and drying the obtained granules to obtain the electrical insulation thermoplastic resin composition; wherein the temperature of a feeding section in the double-screw extruder is 350 ℃, the temperature of a plasticizing shearing section is 365 ℃, the temperature of a machine head is 375 ℃, the rotating speed of a screw is 70r/min, and the rotating speed of grain cutting is 150 r/min.
Examples of the experiments
The electrical insulation thermoplastic resin compositions prepared in the above examples and comparative examples were respectively tested for mechanical properties, electrical insulation properties, heat resistance, thermal expansion coefficient and flame retardancy, and the specific test results are shown in table 1 below.
TABLE 1 test results of examples and comparative examples
The data in the table show that the electrical insulation thermoplastic resin composition provided by the invention has excellent mechanical property, electrical insulation property, flame retardant property and heat resistance, low thermal expansion coefficient and excellent comprehensive performance, and can meet the application requirements under complex working conditions such as large capacity, high field strength, high mechanical load and high temperature field.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the spirit or scope of the invention.
Claims (10)
1. An electrical insulation thermoplastic resin composition is characterized by comprising the following raw materials in parts by weight: 40-70 parts of polyimide; 10-40 parts of polyphenylene sulfide; 15-40 parts of silicon powder and 0.45-1.2 parts of coupling agent.
2. The electrically insulating thermoplastic resin composition according to claim 1, wherein said polyimide is a thermoplastic polyimide.
3. The electrically insulating thermoplastic resin composition as claimed in claim 1 or 2, wherein said polyphenylene sulfide is a linear polyphenylene sulfide.
4. The electrically insulating thermoplastic resin composition according to any one of claims 1 to 3, wherein said fine silica powder is a molten fine silica powder;
the median particle diameter D50 of the silicon micropowder is 5-30 um.
5. The electrical insulating thermoplastic resin composition of any one of claims 1 to 4, wherein the coupling agent is at least one of silane coupling agents KH550, KH560, KH570, KH580 and KH 602.
6. The electrically insulating thermoplastic resin composition according to any one of claims 1 to 5, wherein the mass ratio of the polyimide to the polyphenylene sulfide is 1.8 to 4.0: 1.
7. The method for producing an electrical insulating thermoplastic resin composition as claimed in any one of claims 1 to 6, comprising the steps of:
activating the silicon micropowder by using a coupling agent;
and uniformly mixing the activated coupling agent, polyimide and polyphenylene sulfide, and then extruding, granulating and drying to obtain the electrical insulation thermoplastic resin composition.
8. The method according to claim 7, wherein the activating treatment of the fine silica powder with the coupling agent comprises mixing the coupling agent and the fine silica powder uniformly and drying the mixture.
9. The preparation method according to claim 7 or 8, wherein the extrusion granulation adopts a twin-screw extruder, and the process parameters of the twin-screw extruder comprise: the temperature of the feeding section is 340-.
10. Use of the electrically insulating thermoplastic resin composition as defined in any one of claims 1 to 6 or the electrically insulating thermoplastic resin composition obtained by the process for the preparation of the electrically insulating thermoplastic resin composition as defined in any one of claims 7 to 9 in high voltage insulation parts or high power chip molding.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022233117A1 (en) * | 2021-05-07 | 2022-11-10 | 青岛科技大学 | Thermoplastic special engineering plastic pps/pi alloy material and preparation method therefor |
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| US4017555A (en) * | 1976-06-21 | 1977-04-12 | Alvarez Robert T | Polyalloy of polyphenylene sulfide and polyimide |
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| US20180025957A1 (en) * | 2015-02-25 | 2018-01-25 | Toray Industries, Inc. | Polyphenylene sulfide resin composition, molded product formed therefrom and method of producing semiconductor package |
| CN108359238A (en) * | 2018-02-28 | 2018-08-03 | 佛山慧创正元新材料科技有限公司 | The preparation method of high temperature resistant compound polyimide dielectric material |
| CN109705576A (en) * | 2018-12-27 | 2019-05-03 | 中广核高新核材科技（苏州）有限公司 | A kind of wear-resistant self-lubricating thermoplastic polyimide composite material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4017555A (en) * | 1976-06-21 | 1977-04-12 | Alvarez Robert T | Polyalloy of polyphenylene sulfide and polyimide |
| CN103087524A (en) * | 2013-03-04 | 2013-05-08 | 四川华通特种工程塑料研究中心有限公司 | Polyphenyl thioether sheet with electrical insulation properties and preparation method thereof |
| US20180025957A1 (en) * | 2015-02-25 | 2018-01-25 | Toray Industries, Inc. | Polyphenylene sulfide resin composition, molded product formed therefrom and method of producing semiconductor package |
| CN108359238A (en) * | 2018-02-28 | 2018-08-03 | 佛山慧创正元新材料科技有限公司 | The preparation method of high temperature resistant compound polyimide dielectric material |
| CN109705576A (en) * | 2018-12-27 | 2019-05-03 | 中广核高新核材科技（苏州）有限公司 | A kind of wear-resistant self-lubricating thermoplastic polyimide composite material and preparation method thereof |
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| WO2022233117A1 (en) * | 2021-05-07 | 2022-11-10 | 青岛科技大学 | Thermoplastic special engineering plastic pps/pi alloy material and preparation method therefor |
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