CN113061316B - Graphite whisker filled ABS composition and preparation method thereof - Google Patents
Graphite whisker filled ABS composition and preparation method thereof Download PDFInfo
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- CN113061316B CN113061316B CN202010000306.2A CN202010000306A CN113061316B CN 113061316 B CN113061316 B CN 113061316B CN 202010000306 A CN202010000306 A CN 202010000306A CN 113061316 B CN113061316 B CN 113061316B
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- 239000000203 mixture Substances 0.000 title claims abstract description 56
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 43
- 239000010439 graphite Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 22
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 22
- 238000002844 melting Methods 0.000 claims abstract description 5
- 230000008018 melting Effects 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 34
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 9
- 238000005516 engineering process Methods 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 238000002156 mixing Methods 0.000 abstract description 8
- 238000001125 extrusion Methods 0.000 abstract description 2
- 239000003963 antioxidant agent Substances 0.000 abstract 1
- 230000003078 antioxidant effect Effects 0.000 abstract 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 27
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 241000208181 Pelargonium Species 0.000 description 1
- IUHFWCGCSVTMPG-UHFFFAOYSA-N [C].[C] Chemical group [C].[C] IUHFWCGCSVTMPG-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
- C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The invention discloses a graphite whisker filled ABS composition and a preparation method thereof, wherein the graphite whisker filled ABS composition is prepared from the following components in parts by weight: 100 parts of ABS, 5-10 parts of ASA, 0.5-1 part of polyethylene glycol ether, 5-10 parts of graphite whisker and 264-2 parts of antioxidant. The invention uses polyethylene glycol ether to treat graphite whisker, and adds the graphite whisker into the ABS composition, so that the mechanical property of the ABS composition can be greatly improved. In the preparation process, firstly, the graphite whisker and polyethylene glycol ether are mixed and then other components are added for blending, mainly considering that the polyethylene glycol ether has a low melting point and is close to 60 ℃, and the graphite whisker can be melted and uniformly attached to the surface of the graphite whisker when being stirred at a high speed; when the subsequent extruder is used for melt extrusion, the composition can be ensured to be melted and plasticized uniformly and fully, and the product with excellent performance can be obtained.
Description
Technical Field
The invention belongs to the field of polymer composite materials, and particularly relates to a graphite whisker filled ABS composition and a preparation method thereof.
Background
Graphite whiskers (graphite whiskers), also known as high modulus carbon whiskers, have a stacked structure of a hexagonal network of carbon-carbon atoms. The diameter is 0.2-6 μm, and the length is 50-1 mm. A density of 2.25g/cm3 and a modulus of 97.9GPa; some may be formed in a small spring shape. Excellent in heat resistance, electrical conductivity and flame resistance. The preparation method comprises the following steps: (1) The gas-solid (VS) growth method is that twin crystal beta-SiC is heated to above 1800 ℃ in CO to enable high activity pyrolysis to be piled up and grown on the twin crystal beta-SiC, and then the twin crystal beta-SiC is heated to 2000 ℃; (2) The gas phase reaction process uses low boiling point hydrocarbon as carbon source and argon, nitrogen or superfine transition metal.
Graphite whiskers have poor compatibility with ABS resin matrices, and some have attempted to use KH550 as a treating agent to increase the interfacial bonding ability of the two, but the effect is not ideal.
Disclosure of Invention
The invention aims to provide a graphite whisker filled ABS composition and a preparation method thereof, which are used for solving the problems in the prior art.
The aim of the invention is realized by the following technical scheme:
the graphite whisker filled ABS composition is prepared from the following components in parts by weight:
further, the mass fraction of acrylonitrile in the ABS is 25%, and the mass fraction of styrene is 55%.
Further, the ASA resin has a melt index of 25-30g/10min at 230 ℃ and 2.16 kg.
Further, the melting point of the polyethylene glycol ether is 58-60 ℃.
Further, the diameter of the graphite whisker is 0.5-1 mu m, and the length is 50-200 mu m.
The invention also aims to provide a preparation method of the graphite whisker filled ABS composition, which comprises the following steps:
(1) Adding graphite whisker and polyethylene glycol ether into a mixer according to the proportion, stirring for one time, and uniformly stirring; adding ABS, ASA and antioxidant 264 according to the proportion, and stirring for the second time to obtain a mixture after uniform stirring;
(2) Adding the mixture from a feed inlet of a double-screw extruder, extruding and granulating to prepare the ABS composition.
Further, in the step (1), the stirring speed of the primary stirring is 200-300 rpm, and the stirring time is 1-2 minutes; the stirring speed of the secondary stirring is 150-200 rpm, and the stirring time is 1-2 min.
Further, in the step (2), the processing technology of the twin-screw extruder is as follows: the temperature of the first area is 160-180 ℃, the temperature of the second area is 180-200 ℃, the temperature of the third area is 200-220 ℃, the temperature of the fourth area is 220-230 ℃, the temperature of the fifth area is 220-230 ℃, the temperature of the sixth area is 220-230 ℃, the temperature of the machine head is 220-230 ℃, and the rotating speed frequency of the main machine is 15-35HZ.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention uses polyethylene glycol ether to treat graphite whisker, and adds the graphite whisker into the ABS composition, so that the mechanical property of the ABS composition can be greatly improved.
(2) In the preparation process, firstly, the graphite whisker and polyethylene glycol ether are mixed and then other components are added for blending, mainly considering that the polyethylene glycol ether has a low melting point and is close to 60 ℃, and the graphite whisker can be melted and uniformly attached to the surface of the graphite whisker when being stirred at a high speed; when the subsequent extruder is used for melt extrusion, the composition can be ensured to be melted and plasticized uniformly and fully, and the product with excellent performance can be obtained.
Detailed Description
The invention will be further illustrated with reference to examples. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The types and suppliers of the reagents used in this example are as follows:
ABS is purchased from Taiwan Qimei with the brand pw-757, the mass fraction of acrylonitrile in the ABS is 25%, and the mass fraction of styrene is 55%;
ASA was purchased from Taiwan Qimei under the trade designation pw-957, a melt index of 28g/10min at 230℃under 2.16 kg.
Polyethylene glycol ether is purchased from the Dow chemical, and has a melting point of 58-60 ℃ and a purity of more than 99.9%;
graphite whisker is purchased from Shanghai Pelargonium composite New Material technology Co., ltd;
the above reagents are merely illustrative of the sources and ingredients of the reagents used in the experiments of the invention and are well disclosed and do not represent the inability to practice the invention using other reagents of the same type or provided by other suppliers.
Example 1
(1) Adding 10 parts of graphite whisker and 1 part of polyethylene glycol ether into a mixer to stir at the stirring speed of 300 revolutions per minute for 2 minutes; 100 parts of ABS, 10 parts of ASA and 2 parts of antioxidant 264 are added, and the mixture is mixed for 2 minutes at a mixing speed of 200 revolutions per minute to obtain a mixture.
(2) Adding the mixture from a feed inlet of a double-screw extruder, extruding and granulating to prepare an ABS composition; the processing technology of the double-screw extruder comprises the following steps: the temperature of the first area is 180 ℃, the temperature of the second area is 200 ℃, the temperature of the third area is 220 ℃, the temperature of the fourth area is 230 ℃, the temperature of the fifth area is 230 ℃, the temperature of the sixth area is 230 ℃, the temperature of the machine head is 230 ℃, and the rotating speed frequency of the host machine is 35HZ.
Example 2
(1) Adding 5 parts of graphite whisker and 0.5 part of polyethylene glycol ether into a mixer for stirring at the stirring speed of 200 revolutions per minute for 1 minute; 100 parts of ABS, 5 parts of ASA and 1 part of antioxidant 264 are added, and the mixture is mixed for 1 minute at a mixing speed of 150 revolutions per minute to obtain a mixture.
(2) Adding the mixture from a feed inlet of a double-screw extruder, extruding and granulating to prepare the ABS composition. The processing technology of the double-screw extruder comprises the following steps: the temperature of the first area is 160 ℃, the temperature of the second area is 180 ℃, the temperature of the third area is 200 ℃, the temperature of the fourth area is 220 ℃, the temperature of the fifth area is 220 ℃, the temperature of the sixth area is 220 ℃, the temperature of the machine head is 230 ℃, and the rotating speed frequency of the host machine is 20HZ.
Example 3
(1) Adding 6 parts of graphite whisker and 0.6 part of polyethylene glycol ether into a mixer for stirring at the stirring speed of 250 revolutions per minute for 2 minutes; 100 parts of ABS, 6 parts of ASA and 1.5 parts of antioxidant 264 are added, and the mixture is mixed for 2 minutes at a mixing speed of 180 revolutions per minute to obtain a mixture.
(2) Adding the mixture from a feed inlet of a double-screw extruder, extruding and granulating to prepare an ABS composition; the processing technology of the double-screw extruder comprises the following steps: the temperature of the first area is 170 ℃, the temperature of the second area is 190 ℃, the temperature of the third area is 210 ℃, the temperature of the fourth area is 220 ℃, the temperature of the fifth area is 230 ℃, the temperature of the sixth area is 230 ℃, the temperature of the machine head is 230 ℃, and the rotating speed frequency of the host machine is 30HZ.
Example 4
(1) Adding 7 parts of graphite whisker and 0.7 part of polyethylene glycol ether into a mixer for stirring, wherein the stirring speed is 240 revolutions per minute, and the time is 1 minute; 100 parts of ABS, 7 parts of ASA and 2 parts of antioxidant 264 are added, and the mixture is mixed for 2 minutes at a mixing speed of 160 revolutions per minute to obtain a mixture.
(2) Adding the mixture from a feed inlet of a double-screw extruder, extruding and granulating to prepare an ABS composition; the processing technology of the double-screw extruder comprises the following steps: the temperature of the first area is 170 ℃, the temperature of the second area is 180 ℃, the temperature of the third area is 220 ℃, the temperature of the fourth area is 230 ℃, the temperature of the fifth area is 230 ℃, the temperature of the sixth area is 230 ℃, the temperature of the machine head is 230 ℃, and the rotating speed frequency of the host machine is 35HZ.
Example 5
(1) Adding 8 parts of graphite whisker and 0.8 part of polyethylene glycol ether into a mixer for stirring at a stirring speed of 260 revolutions per minute for 1 minute; 100 parts of ABS, 5 parts of ASA and 2 parts of antioxidant 264 are added, and the mixture is mixed for 2 minutes at a mixing speed of 180 revolutions per minute to obtain a mixture.
(2) Adding the mixture from a feed inlet of a double-screw extruder, extruding and granulating to prepare an ABS composition; the processing technology of the double-screw extruder comprises the following steps: the temperature of the first area is 180 ℃, the temperature of the second area is 200 ℃, the temperature of the third area is 220 ℃, the temperature of the fourth area is 230 ℃, the temperature of the fifth area is 230 ℃, the temperature of the sixth area is 230 ℃, the temperature of the machine head is 230 ℃, and the rotating speed frequency of the host machine is 35HZ.
Comparative example 1
In contrast to example 5. Wherein, the polyethylene glycol ether is replaced by a common coupling agent KH550, and other technical parameters are the same.
Comparative example 2
In contrast to example 5. Wherein, the polyethylene glycol ether is replaced by a common coupling agent KH570, and other technical parameters are the same.
Comparative example 3
In contrast to example 5.
(1) 8 parts of graphite whisker, 0.8 part of polyethylene glycol ether, 100 parts of ABS, 5 parts of ASA and 2 parts of antioxidant 264 are mixed for 2 minutes at a mixing speed of 180 revolutions per minute, so as to obtain a mixture.
(2) Adding the mixture from a feed inlet of a double-screw extruder, extruding and granulating to prepare the ABS composition.
Further, in the step (2), the processing technology of the twin-screw extruder is as follows: the temperature of the first area is 180 ℃, the temperature of the second area is 200 ℃, the temperature of the third area is 220 ℃, the temperature of the fourth area is 230 ℃, the temperature of the fifth area is 230 ℃, the temperature of the sixth area is 230 ℃, the temperature of the machine head is 230 ℃, and the rotating speed frequency of the host machine is 35HZ.
The mechanical property testing method comprises the following steps:
the compositions prepared according to the present invention are injection molded using ASTM standards. The spline dimensions (length x width x thickness) are: the sample strip for testing tensile strength and bending strength is dumbbell-shaped, and is 170mm multiplied by 13mm multiplied by 3.2mm; the notch impact bars were 127mm by 13mm by 3.2mm, V-notch with a notch depth of 1/5.
Tensile strength: the draw speed was 5mm/min as tested by ASTM D638.
Flexural Strength, bending speed was 1.25mm/min as measured by ASTM D790.
Notched impact strength of simply supported beams: tested according to ASTM D6110-2018.
The results of the performance test are shown in Table 1:
TABLE 1 Performance test results
From the table, the polyethylene glycol ether is adopted as an auxiliary agent for treating the graphite whisker, so that the treatment effect is better and better than that of coupling agents KH550 and KH570 commonly used in the market, the dispersibility of the graphite whisker in an ABS resin matrix is greatly enhanced, and the mechanical property of the ABS composition can be greatly improved.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (8)
1. A graphite whisker filled ABS composition characterized in that: the composition is prepared from the following components in parts by weight:
the preparation method of the graphite whisker filled ABS composition comprises the following steps:
(1) Adding graphite whisker and polyethylene glycol ether into a mixer according to the proportion, stirring for one time, and uniformly stirring; adding ABS, ASA and antioxidant 264 according to the proportion, and stirring for the second time to obtain a mixture after uniform stirring;
(2) Adding the mixture from a feed inlet of a double-screw extruder, extruding and granulating to prepare the ABS composition.
2. The graphite whisker filled ABS composition of claim 1, wherein: the mass fraction of acrylonitrile in the ABS is 25%, and the mass fraction of styrene is 55%.
3. The graphite whisker filled ABS composition of claim 1, wherein: the ASA resin has a melt index of 25-30g/10min at 230 ℃ and 2.16 kg.
4. The graphite whisker filled ABS composition of claim 1, wherein: the melting point of the polyethylene glycol ether is 58-60 ℃.
5. The graphite whisker filled ABS composition of claim 1, wherein: the diameter of the graphite whisker is 0.5-1 mu m, and the length is 50-200 mu m.
6. A method of preparing a graphite whisker filled ABS composition according to any one of claims 1 to 5, wherein: the method comprises the following steps:
(1) Adding graphite whisker and polyethylene glycol ether into a mixer according to the proportion, stirring for one time, and uniformly stirring; adding ABS, ASA and antioxidant 264 according to the proportion, and stirring for the second time to obtain a mixture after uniform stirring;
(2) Adding the mixture from a feed inlet of a double-screw extruder, extruding and granulating to prepare the ABS composition.
7. The method of manufacturing according to claim 6, wherein: in the step (1), the stirring speed of the primary stirring is 200-300 rpm, and the stirring time is 1-2 minutes; the stirring speed of the secondary stirring is 150-200 rpm, and the stirring time is 1-2 min.
8. The method of manufacturing according to claim 6, wherein: in the step (2), the processing technology of the double-screw extruder is as follows: the temperature of the first area is 160-180 ℃, the temperature of the second area is 180-200 ℃, the temperature of the third area is 200-220 ℃, the temperature of the fourth area is 220-230 ℃, the temperature of the fifth area is 220-230 ℃, the temperature of the sixth area is 220-230 ℃, the temperature of the machine head is 220-230 ℃, and the rotating speed frequency of the main machine is 15-35HZ.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010000306.2A CN113061316B (en) | 2020-01-02 | 2020-01-02 | Graphite whisker filled ABS composition and preparation method thereof |
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| CN202010000306.2A CN113061316B (en) | 2020-01-02 | 2020-01-02 | Graphite whisker filled ABS composition and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102585429A (en) * | 2011-01-11 | 2012-07-18 | 合肥杰事杰新材料股份有限公司 | Resin material, preparation method and applications of resin material |
| CN109851872A (en) * | 2018-12-27 | 2019-06-07 | 广州弗西林橡塑有限公司 | A kind of high resiliency conductive rubber and preparation method thereof |
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2020
- 2020-01-02 CN CN202010000306.2A patent/CN113061316B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102585429A (en) * | 2011-01-11 | 2012-07-18 | 合肥杰事杰新材料股份有限公司 | Resin material, preparation method and applications of resin material |
| CN109851872A (en) * | 2018-12-27 | 2019-06-07 | 广州弗西林橡塑有限公司 | A kind of high resiliency conductive rubber and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 西鹏.高技术纤维.北京：化学工业出版社,2004,204. * |
| 车剑飞等.复合材料及其工程应用.机械工业出版社,2006,22. * |
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