WO2021097647A1 - 轻质石墨烯复合材料及其制备方法 - Google Patents

轻质石墨烯复合材料及其制备方法 Download PDF

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WO2021097647A1
WO2021097647A1 PCT/CN2019/119372 CN2019119372W WO2021097647A1 WO 2021097647 A1 WO2021097647 A1 WO 2021097647A1 CN 2019119372 W CN2019119372 W CN 2019119372W WO 2021097647 A1 WO2021097647 A1 WO 2021097647A1
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parts
graphene
composite material
graphene composite
lightweight
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林兰花
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南京中弘华飞信息科技有限公司
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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
    • C08K7/00—Use of ingredients characterised by shape
    • 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
    • C08K9/00—Use of pretreated ingredients
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L11/00—Compositions of homopolymers or copolymers of chloroprene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins

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  • the invention belongs to the field of composite materials, and specifically relates to a lightweight graphene composite material and a preparation method thereof.
  • Graphene has a perfect two-dimensional crystal structure, and its crystal lattice is a hexagon surrounded by six carbon atoms. The sigma bond between the carbon atoms makes graphene have excellent mechanical properties and structural rigidity.
  • the lightweight material is a new type of composite material. It uses alkali-resistant glass fiber as the reinforcement, sulfoaluminate low-alkalinity cement as the cementing material, and mixes with suitable base materials to form the base material. It is a new type of inorganic composite material made by the process of extraction, flow slurry and other processes. How to apply graphene to fibers to make composite materials to meet the needs of production and life is a topic worthy of research.
  • the graphene/PBS composite material has a flake-like structure and has a smooth surface structure.
  • the graphene/PBS composite material includes a PBS matrix and graphene powder.
  • the graphene powder is uniformly dispersed in the PBS matrix, and the mass content of graphene in the graphene/PBS composite film is 0.1% to 2.0%.
  • the graphene/PBS composite material has better mechanical properties and heat resistance, and has better elongation at break than PBS materials, and the Young's modulus is significantly reduced.
  • Application No. 2016100967019 discloses a copper-graphene composite material and a preparation method thereof, including graphene and copper, characterized in that the graphene is uniformly distributed in a copper matrix in a sheet-like structure, and the distribution density of the graphene is 100 pieces/cm2 to 3000 pieces/cm2.
  • the graphene content is 0.01% to 0.30 wt%, and the balance is Cu.
  • graphene is added to copper to make a copper-graphene composite material.
  • the copper matrix can be used as a conductive body to make the conductive performance of the composite material close to that of pure copper, while graphene is used as a reinforcing phase, and the tensile strength and yield strength are both Improved; therefore, the copper-graphene composite material can be widely used in the fields of consumer electronics, electrical, aerospace, high-speed rail, lead frame and electronic connector preparation; the preparation method provided by the present invention is suitable for industrialization and large-scale production.
  • the composite material has good electrical conductivity, the graphene is evenly distributed in the copper matrix, and the amount of graphene is high, and the cost is high, and new and improved formulas need to be further sought.
  • the purpose of the present invention is to provide a lightweight graphene composite material and a preparation method thereof.
  • the composite material has light texture, strong bearing capacity, low cost, simple preparation method, and easy industrialization.
  • a lightweight graphene composite material comprising the following components in parts by weight: 20-32 parts of graphene, 30-45 parts of glass fiber, 12-25 parts of neoprene, 5-10 parts of epoxy resin, 8-12 parts of copper powder, 5-8 parts of aluminum powder, 1-3 parts of nano-titanium dioxide, 10-18 parts of attapulgite, 3-5 parts of citric acid, piperazinylpropylmethyldimethoxysilane 12- 20 parts, 18-28 parts of polyvinyl alcohol, 1-3 parts of light carbon black, 1-3 parts of titanate coupling agent.
  • the above-mentioned lightweight graphene composite material includes the following components in parts by weight: 25 parts of graphene, 42 parts of glass fiber, 20 parts of neoprene, 8 parts of epoxy resin, and 10 parts of copper powder. , 6 parts of aluminum powder, 2 parts of nano titanium dioxide, 15 parts of attapulgite, 4 parts of citric acid, 18 parts of piperazinyl propyl methyl dimethoxy silane, 25 parts of polyvinyl alcohol, 2 parts of light carbon black, 2 parts of titanate coupling agent.
  • the preparation method of the above-mentioned lightweight graphene composite material includes the following steps:
  • Step 1 Weigh each component in parts by weight
  • Step 2 Put the attapulgite into a ball mill, grind it to 400-600 mesh, add melted neoprene, stir for 10-15 minutes, add glass fiber, continue to stir, spray dry to obtain glass fiber-loaded attapulgite ;
  • Step 3 Dissolve graphene in deionized water, after ultrasonic treatment, spray drying, and then dissolve in water, add piperazinylpropylmethyldimethoxysilane, copper powder, aluminum powder and nano titanium dioxide, heat and stir , Until the water evaporates to dryness, and modified graphene is obtained;
  • Step 4 After dissolving the modified graphene, adding epoxy resin, citric acid, polyvinyl alcohol, light carbon black and titanate coupling agent after dissolving the modified graphene, stirring, putting it into the mold, and curing lightly. High-quality graphene composite material.
  • the speed of ultrasonic treatment in step 3 is 1000-1200 rpm.
  • the dispersant used in the dispersion treatment in step 4 is acetone.
  • the lightweight material of the present invention improves the mechanical properties of the lightweight graphene composite material by modifying graphene and attapulgite separately, and the modified graphene-copper-aluminum-titania Later, the electrical conductivity has been greatly improved, and it can be used in the preparation of various conductive instruments in the electrical field.
  • a lightweight graphene composite material comprising the following components in parts by weight: 20-32 parts of graphene, 30-45 parts of glass fiber, 12-25 parts of neoprene, 5-10 parts of epoxy resin, 8-12 parts of copper powder, 5-8 parts of aluminum powder, 1-3 parts of nano-titanium dioxide, 10-18 parts of attapulgite, 3-5 parts of citric acid, piperazinylpropylmethyldimethoxysilane 12- 20 parts, 18-28 parts of polyvinyl alcohol, 1-3 parts of light carbon black, 1-3 parts of titanate coupling agent.
  • the preparation method of the above-mentioned lightweight graphene composite material includes the following steps:
  • Step 1 Weigh each component in parts by weight
  • Step 2 Put the attapulgite into a ball mill, grind it to 400 mesh, add melted neoprene, stir for 10 minutes, add glass fiber, and after continuous stirring, spray dry to obtain glass fiber-loaded attapulgite;
  • Step 3 Dissolve the graphene in deionized water, ultrasonically treat it at 1000 rpm, spray and dry it, and then dissolve it in water, add piperazinyl propyl methyl dimethoxy silane, copper powder, aluminum powder and nano titanium dioxide, and heat Stir until the water evaporates to dryness to obtain modified graphene;
  • Step 4 After dissolving the modified graphene and dispersing in acetone, add epoxy resin, citric acid, polyvinyl alcohol, light carbon black and titanate coupling agent, stir, put into the mold, and cure the result. Lightweight graphene composite material.
  • a lightweight graphene composite material including the following components in parts by weight: 25 parts of graphene, 42 parts of glass fiber, 20 parts of neoprene, 8 parts of epoxy resin, 10 parts of copper powder, 6 parts of aluminum powder Parts, 2 parts of nano titanium dioxide, 15 parts of attapulgite, 4 parts of citric acid, 18 parts of piperazinylpropylmethyldimethoxysilane, 25 parts of polyvinyl alcohol, 2 parts of light carbon black, titanate couple 2 parts of coupling agent.
  • the preparation method of the above-mentioned lightweight graphene composite material includes the following steps:
  • Step 1 Weigh each component in parts by weight
  • Step 2 Put the attapulgite clay into a ball mill, grind it to 500 mesh, add melted neoprene, stir for 12 minutes, add glass fiber, and after continuous stirring, spray dry to obtain glass fiber-loaded attapulgite;
  • Step 3 Dissolve graphene in deionized water, sonicated at 1100 rpm, spray dried, and then dissolve in water, add piperazinyl propyl methyl dimethoxy silane, copper powder, aluminum powder and nano titanium dioxide, and heat Stir until the water evaporates to dryness to obtain modified graphene;
  • Step 4 After dissolving the modified graphene and dispersing in acetone, add epoxy resin, citric acid, polyvinyl alcohol, light carbon black and titanate coupling agent, stir, put into the mold, and cure the result. Lightweight graphene composite material.
  • a lightweight graphene composite material comprising the following components in parts by weight: 32 parts of graphene, 45 parts of glass fiber, 25 parts of neoprene, 10 parts of epoxy resin, 12 parts of copper powder, 8 parts of aluminum powder Parts, 3 parts of nano titanium dioxide, 18 parts of attapulgite, 5 parts of citric acid, 20 parts of piperazinyl propyl methyl dimethoxy silane, 28 parts of polyvinyl alcohol, 3 parts of light carbon black, titanate couple Coupling agent 3 parts.
  • the preparation method of the above-mentioned lightweight graphene composite material includes the following steps:
  • Step 1 Weigh each component in parts by weight
  • Step 2 Put the attapulgite into a ball mill, grind it to 500 mesh, add melted neoprene, stir for 10-15 minutes, add glass fiber, and after continuous stirring, spray dry to obtain glass fiber-loaded attapulgite;
  • Step 3 Dissolve graphene in deionized water, sonicated at 1200rpm, spray dried, and then dissolve in water, add piperazinylpropylmethyldimethoxysilane, copper powder, aluminum powder and nano titanium dioxide, and heat Stir until the water evaporates to dryness to obtain modified graphene;
  • Step 4 After dissolving the modified graphene and dispersing in acetone, add epoxy resin, citric acid, polyvinyl alcohol, light carbon black and titanate coupling agent, stir, put into the mold, and cure the result. Lightweight graphene composite material.
  • Example 3 Comparative example 1 Comparative example 2
  • the lightweight material of the present invention has a wide range of materials, the resulting finished product has low density, high compressive strength and high flexural strength.
  • the present invention is not limited to the above-mentioned embodiments, as long as it does not deviate from the scope of the present invention, the present invention can be implemented in various ways.

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)
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Abstract

提供轻质石墨烯复合材料及其制备方法。该复合材料包括以下按照重量份数计的组分：石墨烯20-32份、玻璃纤维30-45份、氯丁橡胶12-25份、环氧树脂5-10份、铜粉8-12份、铝粉5-8份、纳米二氧化钛1-3份、凹凸棒土10-18份、柠檬酸3-5份、哌嗪基丙基甲基二甲氧基硅烷12-20份、聚乙烯醇18-28份、轻质炭黑1-3份、钛酸酯偶联剂1-3份。该复合材料具有提高的力学性能和导电性能，可用于电学领域的各种导电仪器的制备。

Description

[根据细则37.2由ISA制定的发明名称]　轻质石墨烯复合材料及其制备方法 技术领域
本发明属于复合材料领域，具体涉及一种轻质石墨烯复合材料及其制备方法。
背景技术
石墨烯具有完美的二维晶体结构，其晶格由六个碳原子围成的六边形，碳原子之间的σ键使得石墨烯具有优良的力学性质和结构刚性。而轻质材料是一种新型复合材料，它以耐碱玻璃纤维作为增强材、硫铝酸盐低碱度水泥为胶结材并掺入适宜基料构成基材，通过喷射、立模浇铸、挤出、流浆等工艺制成的新型无机复合材料。如何将石墨烯应用于纤维制成复合材料，满足生产生活需要，是一项值得研究的课题。
申请号2016106889244公开一种石墨烯/PBS复合材料，所述石墨烯/PBS复合材料为薄片状结构，且具有光滑的表面结构，所述石墨烯/PBS复合材料包括PBS基体以及石墨烯粉体，所述石墨烯粉体均匀分散于所述PBS基体中，所述石墨烯/PBS复合薄膜中石墨烯的质量含量为0.1％～2.0％。所述石墨烯/PBS复合材料具有更好的力学性能和耐热性能，其相对于PBS材料均具有更好的断裂伸长率，且杨氏模量显著降低。
申请号2016100967019公开了一种铜-石墨烯复合材料及其制备方法，包括石墨烯和铜，其特征在于所述石墨烯以片状结构均布在铜基体中，所述石墨烯的分布密度为100片/厘米2至3000片/厘米2。优选所述石墨烯含量为0.01％～0.30wt％，余量为Cu。本发明在铜中添加石墨烯制成铜-石墨烯复合材料，铜基体可作为导电主体使该复合材料的导电性能接近于纯铜，而石墨烯作为增强相，抗拉强度和屈服强度性能均获得提高；因此该铜-石墨烯复合材料可广泛应用于消费电子、电气、航空航天、高铁、引线框架与电子接插件制备领域；本发明所提供的制备方法适合工业化、规模化生产。虽然该复合材料的导电性好，但石墨烯均布在铜基体中，对石墨烯的用量要求高，成本高，有待进一步寻找新的改进配方。
发明内容
本发明的目的在于提供一种轻质石墨烯复合材料及其制备方法，该复合材料质地轻盈、承重力强、成本低廉的，且制备方法简单，易于产业化。
为解决现有技术问题，本发明采取的技术方案为：
一种轻质石墨烯复合材料，包括以下按照重量份数计的组分：石墨烯20-32份、玻璃纤维30-45份、氯丁橡胶12-25份、环氧树脂5-10份、铜粉8-12份、铝粉5-8份、纳米二氧化钛1-3份、凹凸棒土10-18份、柠檬酸3-5份、哌嗪基丙基甲基二甲氧基硅烷12-20 份、聚乙烯醇18-28份、轻质炭黑1-3份、钛酸酯偶联剂1-3份。
作为改进的是，上述轻质石墨烯复合材料，包括以下按照重量份数计的组分：石墨烯25份、玻璃纤维42份、氯丁橡胶20份、环氧树脂8份、铜粉10份、铝粉6份、纳米二氧化钛2份、凹凸棒土15份、柠檬酸4份、哌嗪基丙基甲基二甲氧基硅烷18份、聚乙烯醇25份、轻质炭黑2份、钛酸酯偶联剂2份。
上述轻质石墨烯复合材料的制备方法，包括以下步骤：
步骤1，按重量份数计称取各组分；
步骤2，将凹凸棒土投入球磨机中，研磨至400-600目，并加入融化的氯丁橡胶，搅拌10-15分钟，加入玻璃纤维，持续搅拌后，喷雾干燥得负载玻璃纤维的凹凸棒土；
步骤3，将石墨烯溶解在去离子水中，超声处理后，喷雾干燥后，再溶于水中，加入哌嗪基丙基甲基二甲氧基硅烷、铜粉、铝粉和纳米二氧化钛，加热搅拌，直至水分蒸干，得到改性石墨烯；
步骤4，将改性石墨烯溶解后，分散处理后，加入环氧树脂、柠檬酸、聚乙烯醇、轻质炭黑和钛酸酯偶联剂，搅拌后，投入模具中，固化处理得轻质石墨烯复合材料。
作为改进的是，步骤3中超声处理的转速为1000-1200rpm。
作为改进的是，步骤4中分散处理用的分散剂为丙酮。
有益效果：
与现有技术相比，本发明轻质材料通过对石墨烯和凹凸棒土分别改性处理后，提高了轻质石墨烯复合材料的力学性能，改性后的石墨烯-铜-铝-二氧化钛后，导电性能已得到很大改进，可用于电学领域的各种导电仪器的制备。
具体实施方式
下面通过具体实施例对本发明作进一步详细介绍。
实施例1
一种轻质石墨烯复合材料，包括以下按照重量份数计的组分：石墨烯20-32份、玻璃纤维30-45份、氯丁橡胶12-25份、环氧树脂5-10份、铜粉8-12份、铝粉5-8份、纳米二氧化钛1-3份、凹凸棒土10-18份、柠檬酸3-5份、哌嗪基丙基甲基二甲氧基硅烷12-20份、聚乙烯醇18-28份、轻质炭黑1-3份、钛酸酯偶联剂1-3份。
上述轻质石墨烯复合材料的制备方法，包括以下步骤：
步骤1，按重量份数计称取各组分；
步骤2，将凹凸棒土投入球磨机中，研磨至400目，并加入融化的氯丁橡胶，搅拌10分钟，加入玻璃纤维，持续搅拌后，喷雾干燥得负载玻璃纤维的凹凸棒土；
步骤3，将石墨烯溶解在去离子水中，超声1000rpm处理后，喷雾干燥后，再溶于水中，加入哌嗪基丙基甲基二甲氧基硅烷、铜粉、铝粉和纳米二氧化钛，加热搅拌，直至水分蒸干，得到改性石墨烯；
步骤4，将改性石墨烯溶解后，丙酮分散处理后，加入环氧树脂、柠檬酸、聚乙烯醇、轻质炭黑和钛酸酯偶联剂，搅拌后，投入模具中，固化处理得轻质石墨烯复合材料。
实施例2
一种轻质石墨烯复合材料，包括以下按照重量份数计的组分：石墨烯25份、玻璃纤维42份、氯丁橡胶20份、环氧树脂8份、铜粉10份、铝粉6份、纳米二氧化钛2份、凹凸棒土15份、柠檬酸4份、哌嗪基丙基甲基二甲氧基硅烷18份、聚乙烯醇25份、轻质炭黑2份、钛酸酯偶联剂2份。
上述轻质石墨烯复合材料的制备方法，包括以下步骤：
步骤1，按重量份数计称取各组分；
步骤2，将凹凸棒土投入球磨机中，研磨至500目，并加入融化的氯丁橡胶，搅拌12分钟，加入玻璃纤维，持续搅拌后，喷雾干燥得负载玻璃纤维的凹凸棒土；
步骤3，将石墨烯溶解在去离子水中，1100rpm超声处理后，喷雾干燥后，再溶于水中，加入哌嗪基丙基甲基二甲氧基硅烷、铜粉、铝粉和纳米二氧化钛，加热搅拌，直至水分蒸干，得到改性石墨烯；
步骤4，将改性石墨烯溶解后，丙酮分散处理后，加入环氧树脂、柠檬酸、聚乙烯醇、轻质炭黑和钛酸酯偶联剂，搅拌后，投入模具中，固化处理得轻质石墨烯复合材料。
实施例3
一种轻质石墨烯复合材料，包括以下按照重量份数计的组分：石墨烯32份、玻璃纤维45份、氯丁橡胶25份、环氧树脂10份、铜粉12份、铝粉8份、纳米二氧化钛3份、凹凸棒土18份、柠檬酸5份、哌嗪基丙基甲基二甲氧基硅烷20份、聚乙烯醇28份、轻质炭黑3份、钛酸酯偶联剂3份。
上述轻质石墨烯复合材料的制备方法，包括以下步骤：
步骤1，按重量份数计称取各组分；
步骤2，将凹凸棒土投入球磨机中，研磨至500目，并加入融化的氯丁橡胶，搅拌10-15 分钟，加入玻璃纤维，持续搅拌后，喷雾干燥得负载玻璃纤维的凹凸棒土；
步骤3，将石墨烯溶解在去离子水中，1200rpm超声处理后，喷雾干燥后，再溶于水中，加入哌嗪基丙基甲基二甲氧基硅烷、铜粉、铝粉和纳米二氧化钛，加热搅拌，直至水分蒸干，得到改性石墨烯；
步骤4，将改性石墨烯溶解后，丙酮分散处理后，加入环氧树脂、柠檬酸、聚乙烯醇、轻质炭黑和钛酸酯偶联剂，搅拌后，投入模具中，固化处理得轻质石墨烯复合材料。
对比例1
除凹凸棒土不进行改性处理外，其余同实施例2。
对比例2
除石墨烯不进行改性处理外，其余同实施例2。
对实施例1-3和对比例1-2的绝缘涂层进行检测，所得数据如下表所示。
  实施例1 实施例2 实施例3 对比例1 对比例2
抗拉强度(MPa) 458 462 428 210 287
导电率(％IACS) 98.2 99.5 99.1 95.2 91.6
屈服强度(MPa) 308.5 315.8 325.1 195.6 197.5
从上述结果可以看出，本发明轻质材料取材广泛、所得成品密度小，抗压强度大、耐折强度高。
另外，本发明不限于上述实施方式，只要在不超出本发明的范围内，可以采取各种方式实施本发明。

Claims (5)

  1. 一种轻质石墨烯复合材料，其特征在于，包括以下按照重量份数计的组分：石墨烯20-32份、玻璃纤维30-45份、氯丁橡胶12-25份、环氧树脂5-10份、铜粉8-12份、铝粉5-8份、纳米二氧化钛1-3份、凹凸棒土10-18份、柠檬酸3-5份、哌嗪基丙基甲基二甲氧基硅烷12-20份、聚乙烯醇18-28份、轻质炭黑1-3份、钛酸酯偶联剂1-3份。
  2. 根据权利要求1所述的轻质石墨烯复合材料，其特征在于，包括以下按照重量份数计的组分：石墨烯25份、玻璃纤维42份、氯丁橡胶20份、环氧树脂8份、铜粉10份、铝粉6份、纳米二氧化钛2份、凹凸棒土15份、柠檬酸4份、哌嗪基丙基甲基二甲氧基硅烷18份、聚乙烯醇25份、轻质炭黑2份、钛酸酯偶联剂2份。
  3. 基于权利要求1或2所述的轻质石墨烯复合材料的制备方法，其特征在于，步骤1，按重量份数计称取各组分；步骤2，将凹凸棒土投入球磨机中，研磨至400-600目，并加入融化的氯丁橡胶，搅拌10-15分钟，加入玻璃纤维，持续搅拌后，喷雾干燥得负载玻璃纤维的凹凸棒土；步骤3，将石墨烯溶解在去离子水中，超声处理后，喷雾干燥后，再溶于水中，加入哌嗪基丙基甲基二甲氧基硅烷、铜粉、铝粉和纳米二氧化钛，加热搅拌，直至水分蒸干，得到改性石墨烯；步骤4，将改性石墨烯溶解后，分散处理后，加入环氧树脂、柠檬酸、聚乙烯醇、轻质炭黑和钛酸酯偶联剂，搅拌后，投入模具中，固化处理得轻质石墨烯复合材料。
  4. 根据权利要求3所述的轻质石墨烯复合材料的制备方法，其特征在于，步骤3中超声处理的转速为1000-1200rpm。
  5. 根据权利要求3所述的轻质石墨烯复合材料的制备方法，其特征在于，步骤4中分散处理用的分散剂为丙酮。
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