CN115873398A - Self-heat-dissipation high-temperature nylon composite material applied to lens module support and preparation method - Google Patents
Self-heat-dissipation high-temperature nylon composite material applied to lens module support and preparation method Download PDFInfo
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- CN115873398A CN115873398A CN202211461457.3A CN202211461457A CN115873398A CN 115873398 A CN115873398 A CN 115873398A CN 202211461457 A CN202211461457 A CN 202211461457A CN 115873398 A CN115873398 A CN 115873398A
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- 239000002131 composite material Substances 0.000 title claims abstract description 88
- 229920001778 nylon Polymers 0.000 title claims abstract description 69
- 239000004677 Nylon Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims description 19
- 229910052582 BN Inorganic materials 0.000 claims abstract description 84
- 229920005989 resin Polymers 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 24
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920006242 ethylene acrylic acid copolymer Polymers 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000002135 nanosheet Substances 0.000 claims description 21
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 20
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 20
- 239000005543 nano-size silicon particle Substances 0.000 claims description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- LIAWCKFOFPPVGF-UHFFFAOYSA-N 2-ethyladamantane Chemical compound C1C(C2)CC3CC1C(CC)C2C3 LIAWCKFOFPPVGF-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 7
- 239000002216 antistatic agent Substances 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical group CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 6
- 229920002292 Nylon 6 Polymers 0.000 claims description 5
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000000413 hydrolysate Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims description 2
- 229920000299 Nylon 12 Polymers 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 6
- XMNDMAQKWSQVOV-UHFFFAOYSA-N (2-methylphenyl) diphenyl phosphate Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C=CC=CC=1)OC1=CC=CC=C1 XMNDMAQKWSQVOV-UHFFFAOYSA-N 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 14
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 8
- 239000003365 glass fiber Substances 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000017525 heat dissipation Effects 0.000 description 4
- 239000004005 microsphere Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000006087 Silane Coupling Agent Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
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- 239000012670 alkaline solution Substances 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
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- 239000000919 ceramic Substances 0.000 description 1
- 239000011246 composite particle Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
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- 238000002425 crystallisation Methods 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
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- 125000000524 functional group Chemical group 0.000 description 1
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- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- -1 polydimethylsiloxane Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a high-temperature nylon composite material applied to self-heat dissipation of a lens module support, which comprises 100-120 parts of nylon resin, 40-60 parts of composite micro-nano h-boron nitride, 5-10 parts of ethylene-acrylic acid copolymer, 3-10 parts of SEBS-g-MA, 2-5 parts of tris (2, 4-di-tert-butylphenyl) phosphite and 5-15 parts of tolyl diphenyl phosphate. The composite micro-nano h-boron nitride composition is selected and modified and is added into the high-temperature nylon composite material as a heat-conducting substance, so that the overall heat-conducting performance is remarkably improved, and the composite micro-nano h-boron nitride composite material has self-heat dissipation performance. The high-temperature nylon composite material prepared by the invention can be widely applied to different working environments.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to a self-heat-dissipation high-temperature nylon composite material applied to a lens module bracket and a preparation method thereof.
Background
The polymer composite material is widely applied to the fields of aerospace, transportation, biomedicine, electronic products, electronic components and the like, and is an indispensable functional material. The well-known melting point of nylon polymer is usually between 295 ℃ and 310 ℃, and the nylon polymer can still maintain excellent mechanical properties and chemical properties in a high-temperature environment, so that the nylon polymer is also a polymer material which is most widely applied. However, polymer materials have poor thermal conductivity and cannot satisfy application environments where heat is generated at relatively high temperatures, and particularly in electronic components, it is necessary to impart not only good heat dissipation properties but also good insulation properties. Polymer composite materials with good heat dissipation and/or thermal conductivity are developed, and usually, heat conduction materials are added into the composite materials; examples include: al (Al) 2 O 3 、AlN、BN、Si 3 N 4 And ceramics such as SiC, carbon nanotubes, carbon fibers, graphene, and the like. Admittedly, the addition of substances having a thermal conductivity does improve the overall thermal conductivity of the composite material, but may also have an adverse effect on the mechanical properties of the material.
In the article "preparation and research of BN/PA66 heat-conducting composite material", the influence of filling boron nitride on the heat-conducting property and the mechanical property of the PA 66/material is researched, and when the addition amount of the boron nitride is 24.8%, the heat-conducting coefficient of the composite material is 0.75W/(m.K); however, the influence of adding BN on the mechanical properties of the composite material is also obvious, the tensile strength and the impact strength of the composite material are reduced along with the increase of the volume fraction of boron nitride, the bending strength tends to increase, the crystallization rate is increased, and the heat deformation temperature is increased, which shows that the rigidity of PA66 is improved but the toughness is reduced by filling boron nitride.
The article 'nano boron nitride and glass fiber composite reinforced nylon 6' researches the influence of pure glass fibers with different contents on the mechanical property of nylon 6 resin, and then the mechanical property and the heat-conducting property of the glass fiber composite material before and after modification are researched by sequentially modifying the surfaces of the glass fibers through dopamine and nano boron nitride. The results show that: when 30% of pure glass fiber is added, the mechanical property of the composite material is best; when the content of the added glass fiber is the same, the mechanical property and the heat-conducting property of the fiber reinforced nylon 6 composite material with the surface modified by the nano boron nitride are greatly improved.
Patent CN111909511A discloses a high-wear-resistance heat-conducting nylon composite material, which comprises the following raw materials in parts by weight: 100 to 110 parts of nylon resin, 10 to 15 parts of hydroxyl-terminated polydimethylsiloxane, 15 to 25 parts of hollow porous carbon microspheres, 10 to 15 parts of nano beta-silicon nitride, 10 to 15 parts of nano magnesium oxide powder, 10 to 15 parts of silicon-aluminum porous microspheres, 5 to 10 parts of nano silicon carbide, 5 to 10 parts of nano silicon dioxide, 0.05 to 0.1 part of lubricant and 0.05 to 0.1 part of antioxidant; the average outer diameter of the hollow porous carbon microsphere is 400-450 nm, the average inner diameter is 320-350 nm, and the diameter of the mesopore is 45-50 nm.
Patent CN110358294A discloses a high-strength heat-conducting nylon composite material, which comprises nylon resin: 100 parts of (A); reinforcing materials: 50-100 parts; heat conductive material: 0.5 to 2.0 portions; flow modifier: 5-20 parts of a solvent; dispersing agent: 0.3 to 0.8 portion; lubricant: 0.1 to 0.6 portion; antioxidant: 0.1 to 0.8 portion; coupling agent: 0.2 to 0.6 portion.
Although the addition of a thermally conductive material is advantageous, the actual situation is more complicated because the influence factor is too numerous and one direction is not clear. Roughly, the specific type (single and/or compound addition), addition amount, shape and size and surface property of the heat-conducting substance can influence the final heat dissipation and/or heat conduction performance of the composite material. Nevertheless, how to prepare high temperature nylon composite materials with high thermal conductivity is still the research direction and focus.
Disclosure of Invention
Based on the needs of the prior art, the invention aims to provide a high-temperature nylon composite material applied to self-heat dissipation of a lens module support and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a be applied to lens module support from radiating high temperature nylon combined material, according to parts by weight, includes the following component preparation:
100 to 120 portions of nylon resin,
40-60 parts of composite micro-nano h-boron nitride,
5 to 10 portions of ethylene-acrylic acid copolymer,
3 to 10 portions of SEBS-g-MA,
2 to 5 portions of phosphorous acid tri (2, 4-di-tert-butylphenyl) ester,
5-15 parts of cresyl diphenyl phosphate.
Further, the self-heat-dissipation high-temperature nylon composite material is prepared from the following components in parts by weight:
105 to 115 portions of nylon resin,
45-55 parts of composite micro-nano h-boron nitride,
7 to 8 portions of ethylene-acrylic acid copolymer,
5 to 7 portions of SEBS-g-MA,
3 to 4 portions of phosphorous acid tri (2, 4-di-tert-butylphenyl) ester,
8-12 parts of cresyl diphenyl phosphate.
Further, the composite nano h-boron nitride is obtained by modifying the surfaces of h-boron nitride micron sheets, h-boron nitride nano sheets and nano silicon nitride powder; the weight ratio of the h-boron nitride micron sheet to the h-boron nitride nano sheet to the nano silicon nitride is 1: (2-3): (2-3); the thickness of the h-boron nitride micron sheet is 0.3-0.5 mu m, and the width-thickness ratio is 100-200; the thickness of the h-boron nitride nanosheet is 20-50 nm, and the width-thickness ratio is 30-40; the grain diameter of the nano silicon nitride powder is 50-100 nm.
Further, the preparation steps of the composite nano h-boron nitride are as follows: (1) Placing the h-boron nitride nanosheets, the h-boron nitride nanosheets and the nano silicon nitride powder into a sodium hydroxide solution, and heating to 80-90 ℃ for dispersing for 30-60 min by adopting ultrasonic waves; (2) Filtering the suspension obtained in the step (1), and washing with deionized water; (3) Dissolving 10-30 parts of 3-aminopropyl 3-ethoxysilane in 100-150 parts of deionized water, heating to 50-60 ℃, and stirring for hydrolysis; (4) Adding the solid component obtained in the step (2) into the hydrolysate obtained in the step (3), heating to 80-90 ℃, and dispersing for 30-60 min by adopting ultrasonic waves; (5) Filtering the suspension obtained in the step (4), and washing with deionized water; drying and grinding the mixture in a drying box at 50-60 ℃ to obtain the composite nano h-boron nitride.
The surface of the composite nano h-boron nitride is hydroxylated by utilizing a silane coupling agent 3-aminopropyl 3-ethoxysilane in hydrolysate, so that the dispersibility of the composite nano h-boron nitride in the subsequent melting process of nylon resin can be improved, and the heat conduction uniformity of the composite material can be effectively ensured; in addition, before entering the hydrolysis solution, the surface is subjected to residual hydroxylation by using an alkaline solution, and ultrasonic dispersion treatment is also beneficial to the dispersion of powder without agglomeration. On the other hand, the group grafted by the silane coupling agent can improve the compatibility of the composite nano h-boron nitride and the nylon resin matrix, and further promotes the heat dissipation performance.
Further, the nylon resin is one or more of nylon 6, nylon 66 and nylon 12.
Further, the high-temperature nylon composite material also comprises 1-3 parts of an antistatic agent; the antistatic agent is an SAS93 antistatic agent.
The invention also provides a preparation method of the high-temperature nylon composite material applied to the self-heat dissipation of the lens module bracket, which comprises the following steps:
(1) Uniformly premixing composite micro-nano h-boron nitride, ethylene-acrylic acid copolymer, SEBS-g-MA, tris (2, 4-di-tert-butylphenyl) phosphite and cresyl diphenyl phosphate according to parts by weight;
(2) Feeding nylon resin from the main feeding of a double-screw extruder, feeding the mixture obtained in the step (1) from the side of the double-screw extruder, melting, mixing, extruding and granulating by the double-screw extruder; and obtaining the self-heat-dissipation high-temperature nylon composite material.
Further, the length-diameter ratio of the double-screw extruder is (45-50): 1. the rotating speed of the screw is controlled to be 300-400 r/min.
Further, the set temperature of the twin-screw extruder is as follows: a first stage: 280-300 ℃, and two-stage: 290-310 ℃ and three sections: 290-310 ℃, four sections: 295-315 ℃ and five sections: 300-320 ℃, six sections: 275-295 ℃ and seven sections: 275-295 ℃ and eight sections: 285-305 ℃, nine stages: 290-310 ℃, head: 300-320 ℃.
Compared with the prior art, the invention has the following beneficial effects: (1) Two heat-conducting substances, namely h-boron nitride and silicon nitride, are compounded to improve the self-heat dissipation of the nylon composite material; meanwhile, the large-size h-boron nitride micron sheet and the small-size h-boron nitride nano sheet are adopted, so that a heat-conducting network can be formed in a nylon matrix by a heat-conducting substance more easily; and the nanometer silicon nitride part enters the micron sheet or the nanometer sheet layer, can be connected with the gap between the h-boron nitride micron sheet and the h-boron nitride nanometer sheet, and can be uniformly dispersed in the nylon matrix, so that the heat conducting property of the nylon matrix is better. (2) The dispersibility of the boron nitride and the silicon nitride is poor, and the composite nano h-boron nitride is subjected to modification treatment, and has functional groups such as hydroxyl groups, amino groups and the like on the surface, so that the compatibility and the dispersibility between the composite nano h-boron nitride and nylon resin are improved when the composite nano h-boron nitride is blended and melted with the nylon resin; the nylon resin is uniformly distributed, so that the whole self-heat dissipation performance of the nylon resin is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1
The utility model provides a be applied to lens module support from radiating high temperature nylon combined material, according to parts by weight, includes the following component preparation:
100 portions of nylon resin,
40 parts of composite micro-nano h-boron nitride,
5 parts of ethylene-acrylic acid copolymer,
3 portions of SEBS-g-MA,
2 parts of tris (2, 4-di-tert-butylphenyl) phosphite,
5 parts of cresyl diphenyl phosphate.
The preparation method of the composite nano h-boron nitride comprises the following steps: (1) Placing the h-boron nitride micron sheet, the h-boron nitride nano sheet and the nano silicon nitride powder in a sodium hydroxide solution, heating to 80 ℃, and dispersing for 30min by adopting ultrasonic waves; (2) Filtering the suspension obtained in the step (1), and washing with deionized water; (3) Dissolving 10 parts of 3-aminopropyl 3-ethoxysilane in 100 parts of deionized water, heating to 50 ℃ and stirring for hydrolysis; (4) Adding the solid component obtained in the step (2) into the hydrolysate obtained in the step (3), heating to 80 ℃, and dispersing for 60min by adopting ultrasonic waves; (5) Filtering the suspension obtained in the step (4), and washing with deionized water; drying and grinding the mixture in a drying box at 50 ℃ to obtain the composite nano h-boron nitride.
Wherein the weight ratio of the h-boron nitride micron sheet to the h-boron nitride nanosheet to the nano silicon nitride is 1:2:2; the thickness of the h-boron nitride micron sheet is 0.3 mu m, and the width-thickness ratio is 100; the thickness of the h-boron nitride nanosheet is 20nm, and the width-thickness ratio is 30; the particle size of the nano silicon nitride powder is 50nm.
The preparation method of the self-heat-dissipation high-temperature nylon composite material comprises the following steps:
(1) Uniformly premixing composite micro-nano h-boron nitride, ethylene-acrylic acid copolymer, SEBS-g-MA, tris (2, 4-di-tert-butylphenyl) phosphite and cresyl diphenyl phosphate according to parts by weight;
(2) Feeding nylon resin from the main feeding of a double-screw extruder, feeding the mixture obtained in the step (1) from the side of the double-screw extruder, and melting, mixing, extruding and granulating the mixture by the double-screw extruder; obtaining the self-heat-dissipation high-temperature nylon composite material.
Further, the length-diameter ratio of the twin-screw extruder is 45: 1. the screw speed control was set to 300r/min.
Further, the set temperature of the twin-screw extruder is as follows: a first stage: 280 ℃ and a second stage: 290 ℃ and three stages: 290 ℃ and four stages: 295 ℃ and five stages: 300 ℃ and six stages: 275 ℃ and seven stages: 275 ℃ and eight stages: 285 ℃ and nine stages: 290 ℃, head: at 300 ℃.
Example 2
The utility model provides a be applied to lens module support from radiating high temperature nylon combined material, according to parts by weight, includes the following component preparation:
120 portions of nylon resin,
60 parts of composite micro-nano h-boron nitride,
10 parts of ethylene-acrylic acid copolymer,
10 portions of SEBS-g-MA,
5 parts of tris (2, 4-di-tert-butylphenyl) phosphite,
15 parts of cresyl diphenyl phosphate.
The preparation method of the composite nano h-boron nitride comprises the following steps: (1) Placing the h-boron nitride micron sheet, the h-boron nitride nano sheet and the nano silicon nitride powder into a sodium hydroxide solution, heating to 90 ℃, and dispersing for 60min by adopting ultrasonic waves; (2) Filtering the suspension obtained in the step (1), and washing with deionized water; (3) Dissolving 30 parts of 3-aminopropyl 3-ethoxysilane in 150 parts of deionized water, heating to 60 ℃, and stirring for hydrolysis; (4) Adding the solid component obtained in the step (2) into the hydrolysate obtained in the step (3), heating to 90 ℃, and dispersing for 30min by adopting ultrasonic waves; (5) Filtering the suspension obtained in the step (4), and washing with deionized water; drying and grinding the mixture in a drying oven at the temperature of 60 ℃ to obtain the composite nano h-boron nitride.
Wherein the weight ratio of the h-boron nitride micron sheet to the h-boron nitride nano sheet to the nano silicon nitride is 1:3:3; the thickness of the h-boron nitride micron sheet is 0.5 mu m, and the width-thickness ratio is 200; the thickness of the h-boron nitride nanosheet is 50nm, and the width-thickness ratio is 40; the particle size of the nano silicon nitride powder is 100nm.
The preparation method of the self-heat-dissipation high-temperature nylon composite material comprises the following steps:
(1) Uniformly premixing composite micro-nano h-boron nitride, ethylene-acrylic acid copolymer, SEBS-g-MA, tris (2, 4-di-tert-butylphenyl) phosphite and cresyl diphenyl phosphate in parts by weight;
(2) Feeding nylon resin from the main feeding of a double-screw extruder, feeding the mixture obtained in the step (1) from the side of the double-screw extruder, melting, mixing, extruding and granulating by the double-screw extruder; obtaining the self-heat-dissipation high-temperature nylon composite material.
Further, the length-diameter ratio of the twin-screw extruder is 50: 1. the screw speed control was set to 300r/min.
Further, the set temperature of the twin-screw extruder is as follows: a first stage: 300 ℃ and a second stage: 310 ℃ and three stages: 310 ℃ and four stages: 315 ℃, five stages: 320 ℃ and six stages: 295 ℃ and seven stages: 295 ℃ and eight sections: 305 ℃ and nine stages: 310 ℃ and a machine head: at 320 ℃.
Example 3
The utility model provides a be applied to lens module support from radiating high temperature nylon combined material, according to parts by weight, includes the following component preparation:
110 portions of nylon resin,
50 parts of composite micro-nano h-boron nitride,
8 parts of ethylene-acrylic acid copolymer,
7 portions of SEBS-g-MA,
4 parts of tris (2, 4-di-tert-butylphenyl) phosphite,
10 parts of cresyl diphenyl phosphate.
The preparation method of the composite nano h-boron nitride comprises the following steps: (1) Placing the h-boron nitride micron sheet, the h-boron nitride nanosheet and the nano silicon nitride powder in a sodium hydroxide solution, heating to 85 ℃, and dispersing for 40min by adopting ultrasonic waves; (2) Filtering the suspension obtained in the step (1), and washing with deionized water; (3) Dissolving 20 parts of 3-aminopropyl 3-ethoxysilane in 130 parts of deionized water, heating to 55 ℃, and stirring for hydrolysis; (4) Adding the solid component obtained in the step (2) into the hydrolysate obtained in the step (3), heating to 85 ℃, and dispersing for 40min by adopting ultrasonic waves; (5) Filtering the suspension obtained in the step (4), and washing with deionized water; drying and grinding the mixture in a drying oven at the temperature of 60 ℃ to obtain the composite nano h-boron nitride.
Wherein the weight ratio of the h-boron nitride micron sheet to the h-boron nitride nano sheet to the nano silicon nitride is 1:2:3; the thickness of the h-boron nitride micron sheet is 0.4 mu m, and the width-thickness ratio is 150; the thickness of the h-boron nitride nanosheet is 30nm, and the width-to-thickness ratio is 35; the particle size of the nano silicon nitride powder is 80nm.
The preparation method of the self-heat-dissipation high-temperature nylon composite material comprises the following steps:
(1) Uniformly premixing composite micro-nano h-boron nitride, ethylene-acrylic acid copolymer, SEBS-g-MA, tris (2, 4-di-tert-butylphenyl) phosphite and cresyl diphenyl phosphate according to parts by weight;
(2) Feeding nylon resin from the main feeding of a double-screw extruder, feeding the mixture obtained in the step (1) from the side of the double-screw extruder, melting, mixing, extruding and granulating by the double-screw extruder; obtaining the self-heat-dissipation high-temperature nylon composite material.
Further, the length-diameter ratio of the twin-screw extruder is 47: 1. the screw speed control was set to 350r/min.
Further, the set temperature of the twin-screw extruder is as follows: a first stage: 290 ℃ and a second stage: 300 ℃ and three stages: 300 ℃ and four stages: 310 ℃ and five stages: 300 ℃ and six stages: 290 ℃ and seven stages: 285 ℃ and eight stages: 295 ℃ and nine stages: 295 ℃, and a machine head: at 310 ℃.
We made the following control tests based on example 3.
Comparative example 1
The comparative example 1 is basically the same as the example 3, and the difference is that the comparative example 1 only adopts h-boron nitride nanosheets to replace the composite micro-nano h-boron nitride in the example 3.
Comparative example 2
The comparative example 2 is basically the same as the example 3, and the difference is that the comparative example 2 only adopts h-boron nitride nanosheets to replace the composite micro-nano h-boron nitride in the example 3.
Comparative example 3
The comparative example 3 is basically the same as the example 3, and the difference is that the comparative example 3 only adopts silicon nitride powder to replace the composite micro-nano h-boron nitride in the example 3.
Comparative example 4
The comparative example 4 is basically the same as the example 3, and the difference is that the comparative example 4 adopts composite micro-nano h-boron nitride, and the composite micro-nano h-boron nitride is only uniformly mixed, but is not subjected to a modification step.
The high temperature nylon composite particles obtained in examples 1 to 3 and comparative examples 1 to 4 were placed in a rectangular mold (20 × 10 × 3 cm), heated to 300 ℃, melted and spread; and (5) cooling and demoulding to obtain the high-temperature-resistant nylon composite material plate.
According to the industry detection standard, the mechanical properties are respectively tested: the tensile strength, the bending strength and the cantilever beam notch impact strength are high; measuring the heat conductivity coefficient by adopting a heat conductivity coefficient tester;
test data are reported in table 1:
TABLE 1
According to the data, the following data are obtained: (1) The high-temperature nylon composite material prepared by the invention has excellent self-heat dissipation performance; the addition of the modified composite micro-nano h-boron nitride is benefited. (2) In comparison, the unmodified composite micro-nano h-boron nitride has poor dispersibility and compatibility with a nylon matrix, so that the heat conductivity is remarkably reduced by about 50 percent; although the thermal conductivity is reduced, the insulating properties are improved. (3) The high-temperature nylon composite material prepared by the invention also has excellent mechanical property and insulating property; the mechanical properties of comparative examples 1 to 4 were reduced, but the reduction was not significant, indicating that the mechanical properties were still good.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (9)
1. The utility model provides a be applied to lens module support from radiating high temperature nylon combined material which characterized in that, according to part by weight, includes that the following component is prepared:
100 to 120 portions of nylon resin,
40-60 parts of composite micro-nano h-boron nitride,
5 to 10 portions of ethylene-acrylic acid copolymer,
3 to 10 portions of SEBS-g-MA,
2 to 5 portions of phosphorous acid tri (2, 4-di-tert-butylphenyl) ester,
5-15 parts of cresyl diphenyl phosphate.
2. The self-heat-dissipation high-temperature nylon composite material as recited in claim 1, comprising the following components in parts by weight:
105 to 115 portions of nylon resin,
45-55 parts of composite micro-nano h-boron nitride,
7 to 8 portions of ethylene-acrylic acid copolymer,
5 to 7 portions of SEBS-g-MA,
3 to 4 portions of phosphorous acid tri (2, 4-di-tert-butylphenyl) ester,
8-12 parts of cresyl diphenyl phosphate.
3. The self-heat-dissipating high-temperature nylon composite material according to any one of claims 1 to 2, wherein the composite nano h-boron nitride is modified by surface modification of h-boron nitride micron sheets, h-boron nitride nano sheets and nano silicon nitride powder; the thickness of the h-boron nitride micron sheet is 0.3-0.5 mu m, and the width-thickness ratio is 100-200; the thickness of the h-boron nitride nanosheet is 20-50 nm, and the width-thickness ratio is 30-40; the grain diameter of the nano silicon nitride powder is 50-100 nm.
4. The self-heat-dissipating high-temperature nylon composite material according to claim 3, wherein the composite nano h-boron nitride is prepared by the following steps: (1) Placing the h-boron nitride nanosheets, the h-boron nitride nanosheets and the nano silicon nitride powder in a sodium hydroxide solution, and heating to 80-90 ℃ to disperse for 30-60 min by adopting ultrasonic waves; (2) Filtering the suspension obtained in the step (1), and washing with deionized water; (3) Dissolving 10-30 parts of 3-aminopropyl 3-ethoxy silane in 100-150 parts of deionized water, heating to 50-60 ℃, and stirring for hydrolysis; (4) Adding the solid component obtained in the step (2) into the hydrolysate obtained in the step (3), heating to 80-90 ℃, and dispersing for 30-60 min by adopting ultrasonic waves; (5) Filtering the suspension obtained in the step (4), and washing with deionized water; drying and grinding the mixture in a drying oven at 50 ℃ to obtain the composite nano h-boron nitride.
5. The self-heat-dissipation high-temperature nylon composite material as claimed in any one of claims 1 to 4, wherein the nylon resin is one or more of nylon 6, nylon 66 and nylon 12.
6. The self-heat-dissipating high-temperature nylon composite material according to any one of claims 1 to 5, further comprising 1 to 3 parts of an antistatic agent; the antistatic agent is an SAS93 antistatic agent.
7. A preparation method of a high-temperature nylon composite material applied to self-heat dissipation of a lens module support is characterized by comprising the following steps:
(1) Uniformly premixing composite micro-nano h-boron nitride, ethylene-acrylic acid copolymer, SEBS-g-MA, tris (2, 4-di-tert-butylphenyl) phosphite and cresyl diphenyl phosphate according to parts by weight;
(2) Feeding nylon resin from the main feeding of a double-screw extruder, feeding the mixture obtained in the step (1) from the side of the double-screw extruder, melting, mixing, extruding and granulating by the double-screw extruder; obtaining the self-heat-dissipation high-temperature nylon composite material.
8. The method for preparing the self-heat-dissipation high-temperature nylon composite material as recited in claim 7, wherein the length-diameter ratio of the twin-screw extruder is (45-50): 1. the rotating speed of the screw is controlled to be 300-400 r/min.
9. The preparation method of the self-heat-dissipation high-temperature nylon composite material as recited in any one of claims 7 to 8, wherein the set temperature of the twin-screw extruder is as follows: a first stage: 280-300 ℃, and two-stage: 290-310 ℃ and three sections: 290-310 ℃, four sections: 295-315 ℃ and five sections: 300-320 ℃, six sections: 275-295 ℃ and seven sections: 275-295 ℃ and eight sections: 285-305 ℃, nine stages: 290-310 ℃, head: 300-320 ℃.
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| CN105295360A (en) * | 2015-10-10 | 2016-02-03 | 惠州市沃特新材料有限公司 | High thermal conductivity flame-retardant nylon composite material and preparation method thereof |
| CN106189209A (en) * | 2016-08-24 | 2016-12-07 | 浙江佳华精化股份有限公司 | Polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds and preparation method thereof |
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| CN105295360A (en) * | 2015-10-10 | 2016-02-03 | 惠州市沃特新材料有限公司 | High thermal conductivity flame-retardant nylon composite material and preparation method thereof |
| CN106189209A (en) * | 2016-08-24 | 2016-12-07 | 浙江佳华精化股份有限公司 | Polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds and preparation method thereof |
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