CN114672155A - 一种聚酰胺复合材料及其制备方法和应用 - Google Patents
一种聚酰胺复合材料及其制备方法和应用 Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 239000004952 Polyamide Substances 0.000 title claims abstract description 36
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- 238000002360 preparation method Methods 0.000 title claims description 6
- 239000011347 resin Substances 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 239000004953 Aliphatic polyamide Substances 0.000 claims abstract description 14
- 229920003231 aliphatic polyamide Polymers 0.000 claims abstract description 14
- -1 methyl triallyl isocyanurate Chemical compound 0.000 claims abstract description 13
- 238000004132 cross linking Methods 0.000 claims abstract description 11
- 239000000945 filler Substances 0.000 claims abstract description 7
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 16
- 239000000347 magnesium hydroxide Substances 0.000 claims description 16
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 16
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- 238000001746 injection moulding Methods 0.000 claims description 10
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
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- RFVNOJDQRGSOEL-UHFFFAOYSA-N 2-hydroxyethyl octadecanoate Chemical group CCCCCCCCCCCCCCCCCC(=O)OCCO RFVNOJDQRGSOEL-UHFFFAOYSA-N 0.000 description 1
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- 241001506304 Kadsura japonica Species 0.000 description 1
- GWFGDXZQZYMSMJ-UHFFFAOYSA-N Octadecansaeure-heptadecylester Natural products CCCCCCCCCCCCCCCCCOC(=O)CCCCCCCCCCCCCCCCC GWFGDXZQZYMSMJ-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- TXQVDVNAKHFQPP-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(CO)(CO)CO TXQVDVNAKHFQPP-UHFFFAOYSA-N 0.000 description 1
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 1
- 239000008116 calcium stearate Substances 0.000 description 1
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- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical group CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
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- FTQWRYSLUYAIRQ-UHFFFAOYSA-N n-[(octadecanoylamino)methyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCNC(=O)CCCCCCCCCCCCCCCCC FTQWRYSLUYAIRQ-UHFFFAOYSA-N 0.000 description 1
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 description 1
- NKBWPOSQERPBFI-UHFFFAOYSA-N octadecyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCCCCCCCCCCCCCCCC NKBWPOSQERPBFI-UHFFFAOYSA-N 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 150000008301 phosphite esters Chemical class 0.000 description 1
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- 238000012545 processing Methods 0.000 description 1
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- 239000011593 sulfur Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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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
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
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- C08K5/20—Carboxylic acid amides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34924—Triazines containing cyanurate groups; Tautomers thereof
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- 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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Abstract
本发明提供了一种聚酰胺复合材料,按重量份计,包括以下组分:短碳链脂肪族聚酰胺树脂100份;导热填料30‑80份;甲基三烯丙基异氰脲酸酯0.01‑15份;所述的聚酰胺复合材料中聚酰胺分子间具有交联结构。本发明通过在导热填料填充短碳链脂肪族聚酰胺树脂中引入甲基三烯丙基异氰脲酸酯进行辐照交联,能够提升聚酰胺复合材料的导热性能。
Description
技术领域
本发明涉及高分子材料技术领域,特别是涉及一种聚酰胺复合材料及其制备方法和应用。
背景技术
高分子材料具有轻质、耐化学腐蚀、易加工成型、电绝缘性能优异、力学及抗疲劳性能优良等特点。然而,绝大数高分子材料热导率极低,是热绝缘体,倘若赋予高分子材料以一定导热性,则会拓宽高分子材料的应用领域,尤其在导热领域的应用。
现有的研究结果表明,提高高分子材料的导热性能的主要途径有合成高导热系数的聚合物和通过高导热无机物对聚合物进行填充。前者如具有良好导热性能的聚吡啶、聚苯胺等,主要通过电子导热机理来提高传热性能,但是导热系数通常低,一般低于1W/mK,并且其价格昂贵。因此,制备高分子聚合物/无机物导热复合材料的研究和应用更为广泛。
但是,如氢氧化镁填充尼龙复合材料可以大幅提升尼龙树脂的导热性能,复合材料的导热性能主要依靠材料内部的导热通路网络的构建完善程度决定。因此,氢氧化镁在复合体系中的添加量往往需要达到50wt%以上,而过高的添加量会带来强度的下降。
发明内容
本发明的目的在于,提供一种聚酰胺复合材料,具有导热性能好、氢氧化镁添加量低的优点。
本发明的另一目的在于,提供上述聚酰胺复合材料的制备方法和应用。
本发明是通过以下技术方案实现的:
一种聚酰胺复合材料,按重量份计,包括以下组分:
短碳链脂肪族聚酰胺树脂 100份;
导热填料 30-80份
甲基三烯丙基异氰脲酸酯 0.01-15份;
所述的聚酰胺复合材料中聚酰胺分子间具有交联结构。
所述的短碳链脂肪族聚酰胺树脂选自PA6、PA46、PA56、PA66中的至少一种。
优选的,所述的短碳链脂肪族聚酰胺树脂选自PA6、PA66中的至少一种。
所述的短碳链脂肪族聚酰胺树脂的重均分子量范围是12000-30000。
所述的导热填料选自氢氧化镁、氢氧化铝、氮化铝、氮化硼、氮化硅、碳化硅、氧化镁、氧化铝中的至少一种。
所述的氢氧化镁的平均粒径为0.5微米-100微米;优选的,平均粒径范围是1微米-15微米。
可以根据实际情况选择是否加入一定量的抗氧剂,助剂的用量可以是0-1份;助剂可以是抗氧剂、润滑剂中的至少一种。
抗氧剂可以是酚类、亚磷酸酯类、二价硫类或空间受阻胺类抗氧剂中的一种或其混合物。
空间受阻胺类抗氧剂可以选自N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺。
润滑剂可以是低分子脂类、金属皂类、硬脂酸复合酯类、酰胺类;其中,低分子脂类为固体石蜡、液体石蜡或低分子聚烯烃蜡,金属皂类为硬脂酸钙、硬脂酸镁、硬脂酸锌或硬脂酸钡,硬酯酸复合酯类为硬脂酸乙二醇酯、硬脂酸甘油酯或硬脂酸季戊四醇酯,酰胺类为芥酸酰胺、甲撑双硬脂酸酰胺或N,N-乙撑双硬脂酸酰胺。
本发明的聚酰胺复合材料的制备方法,包括以下步骤:称取短碳链脂肪族聚酰胺树脂、氢氧化镁、甲基三烯丙基异氰脲酸酯,并将上述各组分投入混合机中进行混合直至均匀,得到预混物;然后将所得预混物投入双螺杆挤出机中进行熔融混合,并挤出造粒,将其进行注塑成型后,进行辐照交联处理,得到无卤阻燃聚酰胺复合材料;其中,双螺杆挤出机的螺杆长径比为40~48:1,螺筒温度为240~300℃,螺杆转速为200~550rpm;注塑温度为250~300℃,注塑压力为55~100 MPa;所述的辐照交联处理的处理过程中采用电子束作为辐射源,辐照剂量为15~25 Mrad;
如有助剂,则与短碳链脂肪族聚酰胺树脂一起混合均匀,再进行后续步骤。
本发明的聚酰胺复合材料的应用,其特征在于,用于制备导热材料。例如照明行业中的LED灯座、电子电器行业中的充电器外壳和交通运输行业中发动机周边部件等对导热及强度要求高的产品中。
本发明与现有技术相比,具有如下有益效果:
本发明通过采用甲基三烯丙基异氰脲酸酯进行辐照交联,能够进一步提升导热填料填充聚酰胺复合材料的导热性能,解决了传统导热树脂中导热填料添加量过高导致强度下降的缺陷。
具体实施方式
下面结合具体实施例对本发明进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进。这些都属于本发明的保护范围。
实施例与对比例所用原材料如下:
PA6:PA6 HY2800A,重均分子量16000-18000,海阳化纤集团;
PA66:PA66 EP158,重均分子量16000-18000,浙江华峰集团;
PA56:PA56,重均分子量13000-18000,上海凯赛生物技术股份有限公司;
PA1012/10T:PA1012/10T ,重均分子量20000-20000,赢创工业集团;
PA1012:PA1012,重均分子量18000-24000,山东广垠新材料有限公司;
甲基三烯丙基异氰脲酸酯:牌号FARIDA H-2,方锐达化学品有限公司;
氢氧化镁A:平均粒径1.5微米,Aitemag® 12FM,江苏艾特克阻燃材料有限公司;
氢氧化镁B:平均粒径15微米,Aitemag® DR-M1,江苏艾特克阻燃材料有限公司;
氢氧化镁C:平均粒径35微米,JMTH-02S,安徽壹石通材料科技股份有限公司;
抗氧剂:N,N'-双-(3-(3,5-二叔丁基-4-羟基苯基)丙酰基)己二胺。
润滑剂:硬脂酸硬脂醇酯,LOXIOL G32,德国科宁。
实施例和对比例聚酰胺复合材料的制备方法:称取聚酰胺树脂、氢氧化镁、甲基三烯丙基异氰脲酸酯、抗氧剂、润滑剂,并将上述各组分投入混合机中进行混合直至均匀,得到预混物;然后将所得预混物投入双螺杆挤出机中进行熔融混合,并挤出造粒,将其进行注塑成型后,进行辐照交联处理,得到无卤阻燃聚酰胺复合材料;其中,双螺杆挤出机的螺杆长径比为44:1,螺筒温度为240~300℃,螺杆转速为400~500rpm;注塑温度为250~300℃,注塑压力为55~100 MPa;所述的辐照交联处理的处理过程中采用电子束作为辐射源,辐照剂量为15~25 Mrad;
测试方法:
(1)导热率测试:按照ISO 22007-1-2009塑料热传导率和热扩散率的测定标准,方法为瞬态平面热源法;
(2)拉伸强度:样品尺寸及测试标准参考ISO 527-2,拉伸速率为50mm/min。干态拉伸强度为标准注塑样条在23℃/50%RH状态调节48h后测试结果;
表1:实施例1-7聚酰胺复合材料各组分含量(重量份)及测试结果
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 | 实施例7 | |
PA6 | 100 | 100 | 100 | 100 | 100 | ||
PA66 | 100 | ||||||
PA56 | 100 | ||||||
甲基三烯丙基异氰脲酸酯 | 5 | 5 | 5 | 8 | 15 | 5 | 5 |
氢氧化镁A | 40 | 40 | 40 | 40 | 40 | 50 | 60 |
抗氧剂 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
润滑剂 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
导热率(W(m<sup>-1</sup>k<sup>-1</sup>)) | 1.2 | 1.2 | 1.1 | 1.3 | 1.4 | 1.2 | 1.4 |
拉伸强度(MPa | 92 | 98 | 88 | 96 | 97 | 94 | 96 |
由实施例1-3可知,短碳链聚酰胺优选PA6和PA66。
表2:实施例8-11聚酰胺复合材料各组分含量(重量份)及测试结果
实施例8 | 实施例9 | 实施例10 | 实施例11 | |
PA6 | 100 | 100 | 100 | 100 |
甲基三烯丙基异氰脲酸酯 | 5 | 5 | 5 | 8 |
氢氧化镁A | 80 | 40 | ||
氢氧化镁B | 50 | |||
氢氧化镁C | 50 | |||
抗氧剂 | 0.1 | 0.1 | 0.1 | |
润滑剂 | 0.1 | 0.1 | 0.1 | |
导热率(W(m<sup>-1</sup>k<sup>-1</sup>)) | 1.6 | 1.2 | 1.2 | 1.5 |
拉伸强度(MPa) | 101 | 92 | 90 | 90 |
由实施例6/10/11可知,优选平均粒径为1-15微米的导热填料。
表3:对比例聚酰胺复合材料各组分含量(重量份)及测试结果
对比例1 | 对比例2 | 对比例3 | |
PA6 | 100 | ||
PA1012/10T | 100 | ||
PA1012 | 100 | ||
甲基三烯丙基异氰脲酸酯 | 5 | 5 | |
氢氧化镁A | 40 | 40 | 40 |
抗氧剂 | 0.1 | 0.1 | 0.1 |
润滑剂 | 0.1 | 0.1 | 0.1 |
导热率(W(m<sup>-1</sup>k<sup>-1</sup>)) | 0.8 | 0.9 | 1.0 |
拉伸强度(MPa | 93 | 88 | 85 |
由实施例1和对比例1可知,交联结构能够提升导热率。
由对比例2/3可知,半芳香聚酰胺或长碳链聚酰胺不能实现提高导热率的技术效果。
Claims (9)
1.一种聚酰胺复合材料,其特征在于,按重量份计,包括以下组分:
短碳链脂肪族聚酰胺树脂 100份;
导热填料 30-80份
甲基三烯丙基异氰脲酸酯 0.01-15份;
所述的聚酰胺复合材料中聚酰胺分子间具有交联结构。
2. 根据权利要求1所述的聚酰胺复合材料,其特征在于,所述的短碳链脂肪族聚酰胺树脂选自PA6、PA 46、PA 56、PA66中的至少一种。
3.根据权利要求2所述的聚酰胺复合材料,其特征在于,所述的短碳链脂肪族聚酰胺树脂选自PA6、PA66中的至少一种。
4.根据权利要求1所述的聚酰胺复合材料,其特征在于,所述的短碳链脂肪族聚酰胺树脂的重均分子量范围是12000-30000。
5.根据权利要求1所述的聚酰胺复合材料,其特征在于,所述的导热填料选自氢氧化镁、氢氧化铝、氮化铝、氮化硼、氮化硅、碳化硅、氧化镁、氧化铝中的至少一种。
6.根据权利要求1所述的聚酰胺复合材料,其特征在于,所述的导热填料的平均粒径为0.5微米-100微米;优选的,平均粒径范围是1微米-15微米。
7.根据权利要求1所述的聚酰胺复合材料,其特征在于,按重量份计,还包括0-1份的助剂,所述的助剂选自抗氧剂、润滑剂中的至少一种。
8. 权利要求1-6任一项所述的聚酰胺复合材料的制备方法,其特征在于,包括以下步骤:称取短碳链脂肪族聚酰胺树脂、导热填料、甲基三烯丙基异氰脲酸酯,并将上述各组分投入混合机中进行混合直至均匀,得到预混物;然后将所得预混物投入双螺杆挤出机中进行熔融混合,并挤出造粒,将其进行注塑成型后,进行辐照交联处理,得到无卤阻燃聚酰胺复合材料;其中,双螺杆挤出机的螺杆长径比为40~48:1,螺筒温度为240~300℃,螺杆转速为200~550rpm;注塑温度为250~300℃,注塑压力为55~100 MPa;所述的辐照交联处理的处理过程中采用电子束作为辐射源,辐照剂量为15~25 Mrad;
如有助剂,则与短碳链脂肪族聚酰胺树脂一起混合均匀,再进行后续步骤。
9.权利要求1-6任一项所述的聚酰胺复合材料的应用,其特征在于,制备导热材料。
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