CN110791095B - Polyphenylene sulfide composite material and preparation method and application thereof - Google Patents
Polyphenylene sulfide composite material and preparation method and application thereof Download PDFInfo
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- CN110791095B CN110791095B CN201810866394.7A CN201810866394A CN110791095B CN 110791095 B CN110791095 B CN 110791095B CN 201810866394 A CN201810866394 A CN 201810866394A CN 110791095 B CN110791095 B CN 110791095B
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- polyphenylene sulfide
- composite material
- sulfide composite
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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
- 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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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
Abstract
The invention provides a polyphenylene sulfide composite material and a preparation method thereof, belonging to the field of modified plastics. The paint comprises the following components in percentage by mass: 20-40% of polyphenylene sulfide, 5-20% of polyamide, 0-60% of a carbonization inhibitor, 0.3-1.2% of gamma-glycidyl ether oxypropyl trimethoxysilane, 0.1-1.0% of n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, 0.1-1.0% of pentaerythritol stearate and 0-30% of chopped glass fiber; wherein the content of the carbonization inhibitor is not 0, and the carbonization inhibitor comprises one or more of magnesium hydroxide, aluminum hydroxide, calcium borate and zinc borate; the sum of the mass percentages of the components is 100%. According to the invention, one or more of magnesium hydroxide, aluminum hydroxide, calcium borate and zinc borate are used as a carbonization inhibitor, and the CTI of the polyphenylene sulfide composite material is improved by using the carbonization inhibitor.
Description
Technical Field
The invention relates to the technical field of modified plastics, in particular to a polyphenylene sulfide composite material and a preparation method and application thereof.
Background
Polyphenylene Sulfide (PPS) has outstanding thermal stability and flame retardant property, excellent chemical resistance, creep resistance, electrical insulation property and processing formability, is a first special engineering plastic and has wide application in the field of electronics and electricity, but certain defects of the PPS affect further application of the PPS.
The relative tracking index (CTI) of the PPS composite material obtained by modifying common polyphenylene sulfide is smaller and about 150V, the CTI of the PPS composite material obtained by compounding the PPS composite material with glass fiber minerals is about 220V, and the application of the PPS composite material in the field with high requirements cannot be met, for example, in Chinese patent CN 104194337A, a glycidyl ester blend grafted by polyethylene and ethylene-glycidyl methacrylate or polyolefin elastomer is used as an impact modifier to improve the impact property and CTI of PPS, but the CTI is not more than 200V at most.
Disclosure of Invention
In view of the above, the present invention aims to provide a polyphenylene sulfide composite material, and a preparation method and an application thereof. The polyphenylene sulfide composite material provided by the invention is added with the carbonization inhibitor, so that the CTI of the polyphenylene sulfide composite material is improved.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a polyphenylene sulfide composite material which comprises the following components in percentage by mass:
wherein the content of the carbonization inhibitor is not 0, and the carbonization inhibitor comprises one or more of magnesium hydroxide, aluminum hydroxide, calcium borate and zinc borate;
the sum of the mass percentages of the components is 100%.
Preferably, the paint comprises the following components in percentage by mass:
preferably, the polyamide comprises one or more of PA6, PA66, PA6T, PA9T, PPA and PA 12.
The invention also provides a preparation method of the polyphenylene sulfide composite material, which comprises the following steps:
(1) mixing polyphenylene sulfide, polyamide, a carbonization inhibitor, gamma-glycidyl ether oxypropyltrimethoxysilane, n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and pentaerythritol stearate to obtain a premix;
(2) and (2) extruding the premix obtained in the step (1) and the chopped glass fiber by a double-screw extruder to obtain the polyphenylene sulfide composite material.
Preferably, the step (2) further comprises cooling and pelletizing after extrusion.
Preferably, the temperature of each zone of the twin-screw extruder in the step (2) is 280-290 ℃, 290-300 ℃, 300-310 ℃, 290-300 ℃, 285-295 ℃, 280-290 ℃, 290-300 ℃ and 300-310 ℃ in sequence.
Preferably, the head temperature of the twin-screw extruder in the step (2) is 305-315 ℃.
Preferably, the mixing time in the step (1) is 2-3 min.
The invention also provides the application of the polyphenylene sulfide composite material in the technical scheme or the polyphenylene sulfide composite material prepared by the preparation method in the technical scheme in the fields of automobiles and electronic and electric appliances.
The invention provides a polyphenylene sulfide composite material which comprises the following components in percentage by mass: 20-40% of polyphenylene sulfide, 5-20% of polyamide, 0-60% of a carbonization inhibitor, 0.3-1.2% of gamma-glycidyl ether oxypropyl trimethoxysilane, 0.1-1.0% of n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, 0.1-1.0% of pentaerythritol stearate and 0-30% of chopped glass fiber; wherein the content of the carbonization inhibitor is not 0, and the carbonization inhibitor comprises one or more of magnesium hydroxide, aluminum hydroxide, calcium borate and zinc borate; the sum of the mass percentages of the components is 100%. According to the invention, one or more of magnesium hydroxide, aluminum hydroxide, calcium borate and zinc borate are used as a carbonization inhibitor, and the carbonization inhibitor can rapidly absorb heat generated during conduction and release the heat, so that the resin carbonization is inhibited, the carbon content is kept not to be increased, and the content of polyphenylene sulfide is reduced by adding the polyamide and the carbonization inhibitor, so that the carbon content is reduced, and the CTI (comparative tracking index) is improved. The data of the examples show that the CTI of the polyphenylene sulfide composite material provided by the invention is as high as 300V, even more than 600V.
Detailed Description
The invention provides a polyphenylene sulfide composite material which comprises the following components in percentage by mass:
wherein the content of the carbonization inhibitor is not 0, and the carbonization inhibitor comprises one or more of magnesium hydroxide, aluminum hydroxide, calcium borate and zinc borate;
the sum of the mass percentages of the components is 100%.
In the invention, the polyphenylene sulfide composite material preferably comprises the following components in percentage by mass:
in the present invention, the polyamide preferably comprises one or more of PA6, PA66, PA6T, PA9T, PPA and PA 12. When the polyamide is preferably a mixture, the invention does not specifically limit the type and amount of the polyamide in the mixture, and any ratio of the mixture may be used. The sources of the PA6, PA66, PA6T, PA9T, PPA and PA12 are not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used.
In the present invention, the number average molecular weight of the polyphenylene sulfide is preferably 30000 to 80000, more preferably 30000 to 50000.
In the invention, the carbonization inhibitor can rapidly absorb heat generated during conduction and release the heat, so that the resin carbonization is inhibited, the carbon content is kept not to be increased, and meanwhile, the content of polyphenylene sulfide is reduced by adding the polyamide and the carbonization inhibitor, so that the carbon content is reduced, and the CTI is improved. When the carbonization inhibitor is preferably a mixture, the invention does not specifically limit the kind and amount of the carbonization inhibitor in the mixture, and the mixture may be used in any proportion.
In the invention, the chopped length of the chopped glass fiber is preferably 2-5 mm, and more preferably 3-4.5 mm.
The invention also provides a preparation method of the polyphenylene sulfide composite material, which comprises the following steps:
(1) mixing polyphenylene sulfide, polyamide, a carbonization inhibitor, gamma-glycidyl ether oxypropyltrimethoxysilane, n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and pentaerythritol stearate to obtain a premix;
(2) and (2) extruding the premix obtained in the step (1) and the chopped glass fiber by a double-screw extruder to obtain the polyphenylene sulfide composite material.
The preparation method comprises the steps of mixing polyphenylene sulfide, polyamide, a carbonization inhibitor, gamma-glycidyl ether oxypropyltrimethoxysilane, n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and pentaerythritol stearate to obtain the premix. The adding sequence of the polyphenylene sulfide, the polyamide, the carbonization inhibitor, the gamma-glycidyl ether oxypropyl trimethoxy silane, the n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and the pentaerythritol stearate is not particularly limited, and the adding sequence known by the technicians in the field can be adopted. The mixing method of the present invention is not particularly limited, and a mixing method known to those skilled in the art may be used. In the invention, the mixing time is preferably 2-3 min. In the present invention, the mixing is preferably carried out in a high-speed mixer.
After the premix is obtained, the premix and the chopped glass fiber are extruded by a double-screw extruder to obtain the polyphenylene sulfide composite material.
In the present invention, the premix is preferably fed from a main feed loss-in-weight scale, and the chopped glass fibers are preferably fed from a side feed loss-in-weight scale.
In the invention, the temperature of each zone of the double-screw extruder is preferably 280-290 ℃, 290-300 ℃, 300-310 ℃, 290-300 ℃, 285-295 ℃, 280-290 ℃, 290-300 ℃ and 300-310 ℃ in sequence.
The present invention is not limited to any particular heating rate for heating to the temperature in each zone of the twin-screw extruder, and the heating rate known to those skilled in the art may be used.
In the invention, the head temperature of the double-screw extruder is preferably 305-315 ℃.
In the present invention, it is also preferable to include cooling pellets after the extrusion. The specific manner of cooling the pellets in the present invention is not particularly limited, and the cooling and pelletizing manner known to those skilled in the art may be used.
The invention also provides the application of the polyphenylene sulfide composite material in the technical scheme in the fields of automobiles and electronic and electric appliances.
In the present invention, the application preferably includes the connector in automobiles and electronic appliances which have requirements on CTI.
In order to further illustrate the present invention, the polyphenylene sulfide composite material provided by the present invention, the preparation method and the application thereof are described in detail below with reference to the examples, but they should not be construed as limiting the scope of the present invention.
Example 1:
the polyphenylene sulfide composite material comprises the following components in percentage by mass: 24 percent of polyphenylene sulfide (the number average molecular weight is 30000), 37.8 percent of magnesium hydroxide, 1.0 percent of gamma-glycidyl ether oxypropyl trimethoxy silane, 0.6 percent of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, 0.6 percent of pentaerythritol stearate and 25.0 percent of chopped glass fiber (the length is 2 mm).
Putting polyphenylene sulfide resin, polyamide PA6, magnesium hydroxide, gamma-glycidyl ether oxypropyltrimethoxysilane, n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and pentaerythritol stearate into a high-speed mixer in proportion for premixing for 2min to form a premix;
feeding the premix from a main feeding weightlessness scale, feeding the chopped glass fiber from a side feeding weightlessness scale, extruding by a double-screw extruder, cooling and granulating to form the polyphenylene sulfide composite material, wherein the temperatures of all zones of the extruder are 280-290 ℃, 290-300 ℃, 300-310 ℃, 290-300 ℃, 285-295 ℃, 280-290 ℃, 290-300 ℃ and 300-310 ℃ in sequence, and the temperature of a machine head is 305-305 ℃.
The CTI (IEC60112) of the polyphenylene sulfide composite material prepared in example 1 is detected to be more than 600V.
Example 2:
the polyphenylene sulfide composite material comprises the following components in percentage by mass: 25 percent of polyphenylene sulfide, 610 percent of polyamide PA, 32.8 percent of mixture (1:1) of zinc borate and magnesium hydroxide, 1.0 percent of gamma-glycidyl ether oxypropyl trimethoxy silane, 0.6 percent of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, 0.6 percent of pentaerythritol stearate and 30.0 percent of chopped glass fiber.
The preparation method is the same as that of example 1.
The CTI (IEC60112) of the polyphenylene sulfide composite material prepared in example 2 was determined to be 500V.
Example 3:
the polyphenylene sulfide composite material comprises the following components in percentage by mass: 33.8 percent of polyphenylene sulfide, 65 percent of polyamide PA, 34.0 percent of magnesium hydroxide, 1.0 percent of gamma-glycidoxypropyltrimethoxysilane, 0.6 percent of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, 0.6 percent of pentaerythritol stearate and 25.0 percent of chopped glass fiber.
The preparation method is the same as that of example 1.
The CTI (IEC60112) of the polyphenylene sulfide composite material prepared in example 3 was found to be 300V.
Example 4:
the polyphenylene sulfide composite material prepared in example 4 was tested to have a CTI (IEC60112) of 270V, as in example 3, except that magnesium hydroxide was replaced with calcium borate.
Comparative example 1:
the polyphenylene sulfide composite material comprises the following components in percentage by mass: 57.8 percent of polyphenylene sulfide, 1.0 percent of gamma-glycidyl ether oxypropyl trimethoxy silane, 0.6 percent of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, 0.6 percent of pentaerythritol stearate and 40.0 percent of chopped glass fiber.
The preparation method is the same as that of example 1.
According to detection, the CTI (IEC60112) of the polyphenylene sulfide composite material prepared in the comparative example 1 is 150V.
Comparative example 2:
the polyphenylene sulfide composite material comprises the following components in percentage by mass: 33.0 percent of polyphenylene sulfide, 24.8 percent of calcium carbonate, 1.0 percent of gamma-glycidyl ether oxypropyl trimethoxy silane, 0.6 percent of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, 0.6 percent of pentaerythritol stearate and 40.0 percent of chopped glass fiber.
The preparation method is the same as that of example 1.
According to detection, the CTI (IEC60112) of the polyphenylene sulfide composite material prepared in the comparative example 2 is 230V.
Therefore, the invention takes one or more of magnesium hydroxide, aluminum hydroxide, calcium borate and zinc borate as the carbonization inhibitor, and the CTI of the polyphenylene sulfide composite material is improved by using the carbonization inhibitor. The data of the examples show that the CTI of the polyphenylene sulfide composite material provided by the invention is as high as 300V, even more than 600V.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (8)
1. The polyphenylene sulfide composite material comprises the following components in percentage by mass:
24 to 38 percent of polyphenylene sulfide
10-11% of polyamide
32.8 to 37.8 percent of carbonization inhibitor
Gamma-glycidoxypropyltrimethoxysilane 1.0%
Beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester 0.6%
Pentaerythritol stearate 0.6%
25-30% of chopped glass fiber;
the carbonization inhibitor comprises one or more of magnesium hydroxide, aluminum hydroxide, calcium borate and zinc borate;
the sum of the mass percentages of the components is 100%.
2. The polyphenylene sulfide composite material of claim 1, wherein the polyamide comprises one or more of PA6, PA66, PA6T, PA9T, PPA, and PA 12.
3. The method for preparing the polyphenylene sulfide composite material according to claim 1 or 2, comprising the steps of:
(1) mixing polyphenylene sulfide, polyamide, a carbonization inhibitor, gamma-glycidyl ether oxypropyltrimethoxysilane, n-octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and pentaerythritol stearate to obtain a premix;
(2) and (2) extruding the premix obtained in the step (1) and the chopped glass fiber by a double-screw extruder to obtain the polyphenylene sulfide composite material.
4. The method of claim 3, wherein the step (2) further comprises cooling and pelletizing after the extruding.
5. The preparation method according to claim 3, wherein the temperatures of the zones of the twin-screw extruder in the step (2) are 280 to 290 ℃, 290 to 300 ℃, 300 to 310 ℃, 290 to 300 ℃, 285 to 295 ℃, 280 to 290 ℃, 290 to 300 ℃ and 300 to 310 ℃ in this order.
6. The production method according to claim 3 or 5, wherein the head temperature of the twin-screw extruder in the step (2) is 305 to 315 ℃.
7. The method according to claim 3, wherein the mixing time in the step (1) is 2 to 3 min.
8. The polyphenylene sulfide composite material as defined in claim 1 or 2 or the polyphenylene sulfide composite material prepared by the preparation method as defined in any one of claims 3 to 7 is applied to the fields of automobiles and electronic appliances.
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| CN201810866394.7A CN110791095B (en) | 2018-08-01 | 2018-08-01 | Polyphenylene sulfide composite material and preparation method and application thereof |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112795191B (en) * | 2020-12-29 | 2022-10-14 | 上海日之升科技有限公司 | High CTI polyphenylene sulfide composite material and preparation method thereof |
| CN113527884A (en) * | 2021-07-12 | 2021-10-22 | 南京真宸科技有限公司 | Polyphenylene sulfide composite material with high CTI (comparative tracking index) |
| CN113402885A (en) * | 2021-07-12 | 2021-09-17 | 南京真宸科技有限公司 | Polyphenylene sulfide composite material with high CTI |
| CN114085522B (en) * | 2021-12-31 | 2024-03-08 | 焦作同辐科技有限责任公司 | High CTI (comparative tracking index) halogen-free flame-retardant glass fiber reinforced PA66/PPO (polyamide-66/Poly-phenylene oxide) composite material and preparation method thereof |
| CN115895261A (en) * | 2022-11-28 | 2023-04-04 | 苏州纳磐新材料科技有限公司 | Polyphenylene sulfide composite material with high CTI performance and preparation method thereof |
| CN116574375A (en) * | 2023-04-24 | 2023-08-11 | 国材(苏州)新材料科技有限公司 | Polyphenylene sulfide resin with high CTI value and CTI value test method |
| CN116426124A (en) * | 2023-05-04 | 2023-07-14 | 国材(苏州)新材料科技有限公司 | High-heat-conduction and heat-dissipation polyphenylene sulfide resin material and preparation method thereof |
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| WO2008123183A1 (en) * | 2007-03-23 | 2008-10-16 | Toray Industries, Inc. | Polyphenylene sulfide resin composition |
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- 2018-08-01 CN CN201810866394.7A patent/CN110791095B/en active Active
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| WO2008123183A1 (en) * | 2007-03-23 | 2008-10-16 | Toray Industries, Inc. | Polyphenylene sulfide resin composition |
| CN103525089A (en) * | 2013-10-18 | 2014-01-22 | 株洲时代新材料科技股份有限公司 | Special packaging material for insulated gate bipolar transistor (IGBT) and preparation method thereof |
| CN104151824A (en) * | 2014-09-02 | 2014-11-19 | 山东赛恩吉新材料有限公司 | High-toughness polyphenylene sulfide elastomer alloy composite material and preparation method thereof |
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