CN115926460A - High-strength high-thermal-conductivity nylon composite material and preparation method thereof - Google Patents
High-strength high-thermal-conductivity nylon composite material and preparation method thereof Download PDFInfo
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- CN115926460A CN115926460A CN202211727741.0A CN202211727741A CN115926460A CN 115926460 A CN115926460 A CN 115926460A CN 202211727741 A CN202211727741 A CN 202211727741A CN 115926460 A CN115926460 A CN 115926460A
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- boron nitride
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- nylon composite
- antioxidant
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- 239000004677 Nylon Substances 0.000 title claims abstract description 39
- 229920001778 nylon Polymers 0.000 title claims abstract description 39
- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 17
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 17
- 229910052582 BN Inorganic materials 0.000 claims abstract description 16
- 239000003365 glass fiber Substances 0.000 claims abstract description 9
- 239000000314 lubricant Substances 0.000 claims abstract description 9
- 229920001721 polyimide Polymers 0.000 claims abstract description 9
- 239000009719 polyimide resin Substances 0.000 claims abstract description 9
- 239000012745 toughening agent Substances 0.000 claims abstract description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 230000010355 oscillation Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 9
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 6
- 239000011258 core-shell material Substances 0.000 description 6
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 229920002302 Nylon 6,6 Polymers 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- PASHVRUKOFIRIK-UHFFFAOYSA-L calcium sulfate dihydrate Chemical compound O.O.[Ca+2].[O-]S([O-])(=O)=O PASHVRUKOFIRIK-UHFFFAOYSA-L 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- BBJZBUKUEUXKDJ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)-n-[1-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoylamino]hexyl]propanamide Chemical compound C=1C(C(C)(C)C)=C(O)C(C(C)(C)C)=CC=1CCC(=O)NC(CCCCC)NC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 BBJZBUKUEUXKDJ-UHFFFAOYSA-N 0.000 description 1
- XAQKFOUWWAKVCH-UHFFFAOYSA-N OP(O)OP(O)O.C(C)(C)(C1=CC=CC=C1)C1=C(C=CC(=C1)C(C)(C)C1=CC=CC=C1)C(O)C(CO)(CO)CO Chemical group OP(O)OP(O)O.C(C)(C)(C1=CC=CC=C1)C1=C(C=CC(=C1)C(C)(C)C1=CC=CC=C1)C(O)C(CO)(CO)CO XAQKFOUWWAKVCH-UHFFFAOYSA-N 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical group CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
The invention discloses a high-strength high-thermal-conductivity nylon composite material and a preparation method thereof, belonging to the technical field of nylon filling materials, and the technical scheme is characterized in that the material comprises 50-70 parts of polyimide resin, 20-30 parts of glass fiber, 3-5 parts of three-dimensional boron nitride, 3-5 parts of aluminum oxide, 3 parts of a toughening agent POE-G, 0.2 part of a main antioxidant, 0.2 part of an auxiliary antioxidant and 0.5 part of a lubricant by weight; compared with the existing nylon composite material, the nylon composite material prepared by the invention has better strength and heat-conducting property.
Description
Technical Field
The invention relates to the technical field of nylon composite materials, in particular to a high-strength high-heat-conductivity nylon composite material and a preparation method thereof.
Background
Nylon materials possess high chemical resistance, processability and heat resistance. Making them particularly suitable for use in the field of high performance demanding electrical/electronic devices and the like. The nylon material has low heat conductivity coefficient, so that the application of the nylon material in a heat dissipation part is limited, and therefore, the nylon material needs to be modified by adding a heat conduction material, and the heat conductivity coefficient of the composite material is improved.
The prior art of thermally conductive modified nylon composites can be referred to the following patent applications.
The Chinese patent application with the application number of CN202210809215.2, which is briefly described as material I below, discloses a high-impact-resistance high-thermal-conductivity nylon composite material and a preparation method thereof, wherein the composite material comprises the following components: nylon resin, a core-shell butyl acrylate grafted maleic anhydride blend, a compound filler and an auxiliary agent; wherein the mass portion of the blend of the nylon resin and the butyl acrylate grafted maleic anhydride with the core-shell structure is 38-38.3%; the mass portion of the compound filler is 60%, and the balance is an auxiliary agent; in the blend of the nylon resin and the butyl acrylate grafted maleic anhydride with the core-shell structure, the ratio of the nylon resin to the butyl acrylate grafted maleic anhydride with the core-shell structure is 85% to 15, the core-shell ratio of the butyl acrylate grafted maleic anhydride with the core-shell structure is 80% to 20, and the proportion of the maleic anhydride in a butyl acrylate shell layer is 3%; the compound filler comprises aluminum oxide, natural crystalline flake graphite and carbon nano tubes; the auxiliary agent comprises an antioxidant and a lubricant.
The Chinese patent application file with the application number of CN202210071362.4, which is briefly described as material II below, discloses a heat-conducting nylon composite material prepared from PA66 heat-conducting composite material powder, wherein the composite material powder comprises the following raw materials in parts by mass: 80-100 parts of phosphogypsum, 1600-2000 parts of distilled water, 80-100 parts of nylon 66 powder, 10-20 parts of multi-walled carbon nano tube, 12-20 parts of concentrated sulfuric acid, 24-40 parts of concentrated nitric acid and the preparation method of PA66 heat-conducting composite material powder comprises the following steps: firstly, uniformly mixing phosphogypsum and distilled water, then adding nylon 66 powder and multi-walled carbon nanotubes, uniformly mixing, then adding concentrated sulfuric acid and concentrated nitric acid, uniformly mixing, stirring at 90-100 ℃ for full reaction, then filtering the hot reaction product to obtain a filtrate, standing the filtrate until the filtrate is cooled to room temperature and fully crystallized, finally filtering to obtain filter residue, and washing and drying the filter residue to obtain the composite material powder.
Disclosure of Invention
One of the purposes of the present invention is to provide a nylon composite material with high strength and high thermal conductivity, which has better strength and thermal conductivity compared with the existing nylon composite material.
The above purpose of the invention is realized by the following technical scheme: the high-strength high-thermal-conductivity nylon composite material comprises, by mass, 50-70 parts of polyimide resin, 20-30 parts of glass fiber, 3-5 parts of three-dimensional boron nitride, 3-5 parts of aluminum oxide, 3 parts of a toughening agent POE-G, 0.2 part of a main antioxidant, 0.2 part of an auxiliary antioxidant and 0.5 part of a lubricant.
One of the purposes of the invention is to provide a preparation method of a high-strength high-thermal-conductivity nylon composite material, which is used for preparing the high-strength high-thermal-conductivity nylon composite material.
The above purpose of the invention is realized by the following technical scheme: a preparation method of a high-strength high-heat-conductivity nylon composite material comprises the following steps:
step S1, weighing polyimide resin, glass fiber, three-dimensional boron nitride, aluminum oxide, a toughening agent, a main antioxidant, an auxiliary antioxidant and a lubricant according to a ratio;
s2, uniformly mixing the polyimide resin and a toughening agent POE-G to form a primary mixed raw material;
uniformly mixing three-dimensional boron nitride, a lubricant, a main antioxidant and an auxiliary antioxidant together to form a mixed auxiliary material; then adding the mixed auxiliary materials into the primary mixed raw materials for uniform mixing;
s3, adding the uniformly mixed raw materials into a double-screw extruder for extrusion, and adding glass fibers from a side feeding port; the temperature of each temperature zone of the extruder is as follows; a first region: 200-240 ℃; a second zone: 230-250 ℃; three zones: 230-250 ℃; and (4) four areas: 235 to 255 ℃; and a fifth zone: 245-255 ℃; a sixth zone: 245-255 ℃; seven areas: 240-250 ℃; and eight regions: 230 to 240 ℃; nine areas: 240-250 ℃; a machine head: 245-255 ℃;
and cooling and granulating the extruded material to obtain the high-strength high-heat-conductivity nylon composite material.
Preferably, the three-dimensional boron nitride is prepared by the following method:
adding boron nitride into water, and carrying out ultrasonic oscillation to form a hydroxylated boron nitride solution;
mixing the hydroxylated boron nitride solution with the PVA solution, stirring and carrying out ultrasonic oscillation treatment on the mixed solution, and uniformly mixing the used solution; and drying the mixed solution to obtain the three-dimensional boron nitride.
Detailed Description
The embodiment is as follows:
examples 1 to 9
Examples 1 to 9 adopt the above-mentioned preparation process, respectively change the component proportions of the polyimide resin, the glass fiber, the three-dimensional boron nitride, the alumina, the polytetrafluoroethylene in the formulation, prepare and obtain 9 kinds of high-strength high-thermal conductivity nylon composite material samples with different component proportions, wherein the mass fractions of the polyimide resin are singly changed in examples 1, 2, 3; examples 1, 4, 5 mass fractions of single-transition glass fibers; examples 1, 6, 7 mass fraction of single transformation three-dimensional boron nitride; examples 1, 8, 9 mass fractions of single-shifted alumina. In examples 1-9, the primary antioxidant was N, N' -bis- (3- (3,5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine; the auxiliary antioxidant is (2,4-dicumylphenyl) pentaerythritol-diphosphite; the lubricant is ethylene bis stearamide.
The component ratios of the high-strength and high-thermal-conductivity nylon composite materials prepared in examples 1 to 9 are specifically shown in table 1.
TABLE 1 EXAMPLES 1-9 high-Strength, high-thermal conductivity Nylon composite component ratios
The unit of data in table 1 is parts by mass.
Comparative example
Comparative example 1
A comparative example is the same process as example 1 except that no three-dimensional boron nitride is added.
Comparative example 2
The comparative example is the same process as example 1 except that no alumina is added.
Comparative example 3
The nylon composite material is prepared by adopting the formula and the preparation method of the material I in the background technology.
Comparative example 4
The nylon composite material is prepared by adopting the formula and the preparation method of the material II in the background technology.
Test method
The high-strength and high-thermal-conductivity nylon composite materials prepared in examples 1 to 9 and the nylon composite materials prepared in comparative examples 1 to 4 were used as test samples, and mechanical properties were measured.
Wherein, the notched impact strength of the cantilever beam is tested according to a method specified in GB/T1843-2008;
the tensile strength is tested according to the method specified in GB/T1040-2018;
the bending strength is tested according to the method specified in GB/T9341-2008;
the flexural modulus is tested according to the method specified in GB/T9341-2008;
the heat conductivity coefficient test is carried out according to the method specified in GB/T3139;
the test results are shown in table 2.
TABLE 2 Performance test data for samples of materials prepared in examples 1-9 and comparative examples 1-4
Combining the data from tables 1 and 2, one can obtain:
compared with the nylon composite material prepared by the conventional method, the nylon composite material prepared by the preparation process has the advantages that the tensile strength, the bending strength and the impact strength are greatly improved, and the variable property cannot be improved on the performance through single component change, so that the effect obtained by the formula is obtained by the synergistic effect of various materials.
Although some specific embodiments of the present invention have been described in detail by way of illustration, it should be understood by those skilled in the art that the above illustration is only for the purpose of illustration and is not intended to limit the scope of the invention. It will be appreciated by those skilled in the art that modifications can be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.
Claims (3)
1. The utility model provides a high strength high heat conduction nylon composite which characterized in that: the composite material comprises, by mass, 50-70 parts of polyimide resin, 20-30 parts of glass fiber, 3-5 parts of three-dimensional boron nitride, 3-5 parts of aluminum oxide, 3 parts of a toughening agent POE-G, 0.2 part of a main antioxidant, 0.2 part of an auxiliary antioxidant and 0.5 part of a lubricant.
2. A preparation method of a high-strength high-thermal-conductivity nylon composite material is characterized by comprising the following steps:
step S1, weighing polyimide resin, glass fiber, three-dimensional boron nitride, alumina, a flexibilizer, a main antioxidant, an auxiliary antioxidant and a lubricant according to a ratio;
s2, uniformly mixing the polyimide resin and a toughening agent POE-G to form a primary mixed raw material;
uniformly mixing three-dimensional boron nitride, a lubricant, a main antioxidant and an auxiliary antioxidant together to form a mixed auxiliary material; then adding the mixed auxiliary materials into the primary mixed raw materials for uniform mixing;
s3, adding the uniformly mixed raw materials into a double-screw extruder for extrusion, and adding glass fibers from a side feeding port; the temperature of each temperature zone of the extruder is as follows; a first region: 200-240 ℃; and a second zone: 230-250 ℃; and (3) three zones: 230-250 ℃; and (4) four areas: 235 to 255 ℃; and a fifth zone: 245-255 ℃; a sixth zone: 245-255 ℃; seven areas: 240-250 ℃; and eight regions: 230 to 240 ℃; nine areas: 240-250 ℃; a machine head: 245-255 ℃;
and cooling and granulating the extruded material to obtain the high-strength high-heat-conductivity nylon composite material.
3. The preparation method of the nylon composite material with high strength and high thermal conductivity according to claim 2, wherein the three-dimensional boron nitride is prepared by the following method:
adding boron nitride into water, and carrying out ultrasonic oscillation to form a hydroxylated boron nitride solution;
mixing the hydroxylated boron nitride solution with the PVA solution, stirring and ultrasonically oscillating the mixed solution, and uniformly mixing the used solution; and drying the mixed solution to obtain the three-dimensional boron nitride.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211727741.0A CN115926460A (en) | 2022-12-30 | 2022-12-30 | High-strength high-thermal-conductivity nylon composite material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211727741.0A CN115926460A (en) | 2022-12-30 | 2022-12-30 | High-strength high-thermal-conductivity nylon composite material and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293452A (en) * | 2015-08-31 | 2016-02-03 | 中国科学院深圳先进技术研究院 | Three-dimensional-structure boron nitride as well as preparation method and application thereof |
| CN113462152A (en) * | 2021-08-05 | 2021-10-01 | 深圳市沃特新材料股份有限公司 | LED lamp cup, insulating and heat-conducting composite material, and preparation method and application thereof |
| CN115028892A (en) * | 2022-06-10 | 2022-09-09 | 安徽建筑大学 | Three-dimensional structure modified boron nitride and preparation method and application thereof |
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- 2022-12-30 CN CN202211727741.0A patent/CN115926460A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293452A (en) * | 2015-08-31 | 2016-02-03 | 中国科学院深圳先进技术研究院 | Three-dimensional-structure boron nitride as well as preparation method and application thereof |
| CN113462152A (en) * | 2021-08-05 | 2021-10-01 | 深圳市沃特新材料股份有限公司 | LED lamp cup, insulating and heat-conducting composite material, and preparation method and application thereof |
| CN115028892A (en) * | 2022-06-10 | 2022-09-09 | 安徽建筑大学 | Three-dimensional structure modified boron nitride and preparation method and application thereof |
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