CN110003577A - 一种go/cnt/iir高导热复合材料制备方法 - Google Patents
一种go/cnt/iir高导热复合材料制备方法 Download PDFInfo
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- CN110003577A CN110003577A CN201910332873.5A CN201910332873A CN110003577A CN 110003577 A CN110003577 A CN 110003577A CN 201910332873 A CN201910332873 A CN 201910332873A CN 110003577 A CN110003577 A CN 110003577A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
- C08J3/21—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase
- C08J3/215—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase at least one additive being also premixed with a liquid phase
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08J2323/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08J2323/22—Copolymers of isobutene; butyl rubber
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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
- 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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- 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
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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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
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- C08K3/02—Elements
- C08K3/04—Carbon
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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
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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
本发明属于橡胶制备技术领域,具体涉及一种GO/CNT/IIR高导热复合材料制备方法,基于干冰易升华的特点,将其引入到氧化石墨烯/碳纳米管/丁基胶乳的混合液中,干冰在遇热时体积瞬间能膨胀600‑800倍,气泡膨胀破裂产生的极大能量,类似于微型爆炸,爆炸冲击波促使胶料分子链断裂,降低胶料的粘度,从而有利于纳米填料的分散。由于干冰升华吸收大量的热,使橡胶分子链骤冷,刚性增加,导致转子的剪切作用力更有效的传导入橡胶内部,使氧化石墨烯团聚体破碎,带动GO和CNT的分散,增大GO、CNT与IIRL中橡胶烃的接触面积,提高GO/CNT/IIR复合材料的导热性能。
Description
技术领域:
本发明属于橡胶制备技术领域,具体涉及一种GO/CNT/IIR高导热复合材料制备方法,以氧化石墨烯(GO)分散液、碳纳米管(CNT)和丁基胶乳(IIRL)为原料,采用干冰膨胀预分散絮凝法制备GO/CNT/IIR复合材料。
背景技术:
随着航空、航天、电子电气等高科技领域的快速发展,橡胶的导热性能越来越受到重视。例如,高性能电子产品的橡胶密封件既要具备优良的导热性能和绝缘性能,又要具备防潮、防尘和减震性能;化学工业生产和废水处理等领域要求热交换器橡胶垫圈具有良好的导热性能、耐高温性能和耐化学腐蚀性能;导热橡胶具备以上优点,使其在导热材料领域备受关注。
氧化石墨烯(GO)是石墨烯的衍生物,是石墨经过氧化后得到的具有原石墨结构中的碳原子杂化类型为sp2碳结构的二维材料。GO具有超薄的片层结构、大的比表面积,其表面含有大量的羟基、羧基等含氧基团,具有优异的力学、热学和电学性能。这些性能使GO在添加到橡胶基体中时,能大幅度提高橡胶基复合材料的力学性能、热学性能、导电性能等多种性能。但是GO的结构特点,导致GO片层极易团聚,不容易分散,极大的影响了GO在橡胶基体中发挥性能的效果。如何使GO在橡胶基体中均匀分散及增强GO与橡胶基体间的界面相互作用是目前要解决的难题之一。
碳纳米管(CNT)作为一维纳米材料,重量轻,六边形结构连接完美,具有许多异常的力学、电学和化学性能。近些年随着碳纳米管及纳米材料研究的深入其广阔的应用前景也不断地展现出来,同时具有优异的力学、热学和电学性能。它作为纳米填料,具有超强的比表面积和特殊的结构。它们可以用来填充橡胶,同时具有优异的物理和机械性能、导电性和导热性。目前,人们已使用这些新型纳米填料来提高橡胶制品的性能,这对橡胶制品的高性能和功能化具有重要意义。考虑到CNT与氧化石墨烯在结构上和物理性质上的相似性,它们在某些情况下可能会产生协同效应。
丁基橡胶是合成橡胶的一种,由异丁烯和少量异戊二烯合成,丁基橡胶的气密性好,还能耐热、耐臭氧、耐老化、耐化学药品,并有吸震和电绝缘性能,对阳光及臭氧具良好的抵抗性,可暴露于动物或植物油或是可氧化的化学物中,一般被应用在制作汽车轮胎以及汽车隔音用品里面,在建筑防水领域,丁基橡胶以环保的名号已经全面普及代替沥青,在橡胶工业中占据重要地位,然而,丁基橡胶的结构特点使其硫化速度慢、互粘性差、与其它橡胶相容性差以及与补强剂之间作用弱,这些缺点制约了丁基橡胶的加工和应用,改善丁基橡胶的性能尤为重要。
干冰是固态的二氧化碳,在6250.5498KPa压力下,把二氧化碳冷凝成无色的液体后在高压下迅速凝固能够得到干冰。二氧化碳常态下是一种无色无味的气体,自然存在于空气中,虽然二氧化碳在空气中的含量相对很小,但它却是人们所认识的最重要的气体之一。干冰极易挥发,能够升华为无毒、无味的,比固体体积大600-800倍的气体二氧化碳。干冰膨胀法最常用于卷烟工业中烟丝的制造工艺,即干冰膨胀烟丝技术,具体工艺为将液态二氧化碳在恒定压力下浸渍烟丝一段时间,然后快速冷却,浸渍在烟草细胞中的液体二氧化碳,在瞬间释放压力后立即用不饱和蒸汽加热烟丝,使固体二氧化碳升华为气态,促使烟草细胞膨胀,干冰气化是烟丝细胞结构膨胀的根本原因。
目前,CNT/橡胶复合材料的制备方法主要包括机械共混法、溶液共混法、熔融共混法和乳液共混法等传统工艺方法。中国专利201510770421.7公开的一种聚甲基苯基硅氧烷-碳纳米管-硅橡胶复合材料,按照下述步骤进行:步骤1:将90-110重量份硅橡胶生胶在温度43-48℃的双辊上,混炼2-5min,使硅橡胶生胶均匀粘辊;步骤2:依次加入30-50重量份白炭黑、8-15重量份二苯基硅二醇、1.5-3重量份多乙烯基硅油,1-5重量份聚甲基苯基硅氧烷非共价修饰碳纳米管和0.4-1重量份过氧化双(2,4-二氯苯甲酰),混炼12-14min,将胶料混炼均匀获得混炼胶;步骤3:将步骤2制备的混炼胶装入模具中,温度为175-185℃,压力5-12MPa的条件下热压9-12min硫化成型,冷却后得到硫化胶片;所述步骤1中,所述硅橡胶生胶为甲基乙烯基硅橡胶;所述步骤2中,聚甲基苯基硅氧烷非共价修饰碳纳米管中,聚甲基苯基硅氧烷上的苯环与碳纳米管间以π-π作用进行复合,并按照下述方法进行制备:步骤1,称取0.5-1.5质量份羧基化碳纳米管超声分散在蒸馏水中,得到羧基化碳纳米管的水相分散液;称取0.5-5.0质量份聚甲基苯基硅氧烷超声分散在无水乙醇中,得到聚甲基苯基硅氧烷的无水乙醇分散液;步骤2,将聚甲基苯基硅氧烷的无水乙醇分散液滴加入羧基化碳纳米管的水相分散液中,冰浴超声处理20-40min后取出,密封静置22-26h后进行抽滤烘干;中国专利201610494634.6公开的一种气相分散的碳纳米管分散体制备碳纳米管/天然橡胶复合材料的方法,依次含有以下步骤:(1)将去离子水与天然橡胶乳液混合制备低浓度天然橡胶乳液,低浓度天然橡胶乳液中固体物含量为0.1%甚至更高;(2)按照所需将定量气相分散的碳纳米管分散体收集物加入到步骤(1)所制得的低浓度天然橡胶乳液中,进行抽真空,抽真空时间为5分钟甚至更长,使得气相分散的碳纳米管分散体收集物浸润到步骤(1)所制得的低浓度天然橡胶乳液中得到预复合产品;(3)按所需浓度比例将适量纯天然橡胶乳液加入到(2)说述的预复合产品中,充分搅拌混合;(4)加入破乳剂进行破乳,经后续进一步加工,制备得碳纳米管/天然橡胶复合材料;中国专利200810224959.8公开的一种碳纳米管-天然橡胶复合材料的制备方法,采用通过天然橡胶的环氧化反应制备的环氧化天然橡胶作为碳纳米管与天然橡胶之间的相容剂,利用环氧化天然橡胶与天然橡胶之间优异的相容性,以及环氧化天然橡胶与碳纳米管之间的化学反应,改善碳纳米管在天然橡胶中的分散效果,增强碳纳米管与天然橡胶之间的相互作用,制备高性能碳纳米管-天然橡胶复合材料;中国专利201310636376.7公开的一种氧化铁修饰碳纳米管—硅橡胶复合材料,按照下述步骤进行:步骤1,将100重量份硅橡胶生胶在温度40—50℃的双辊上,混炼1-10min,使生胶均匀粘辊;步骤2,按顺序加入38—40重量份白炭黑、10—12重量份六甲基二硅氮烷和2—3重量份多乙烯基硅油,混炼10-15min,将胶料混炼均匀;步骤3,加入3—5重量份氧化铁修饰碳纳米管,混炼5-10min,混炼均匀后加入0.5—1重量份2,5-二甲基-2,5-二叔丁基过氧化己烷,混炼10—15min后打卷下片;步骤4,将步骤3所得的混炼胶装入模具,温度160—180℃,压力10—12MPa的条件下热压10—15min硫化成型,冷却后得到硫化胶片;将硫化胶片置于200℃环境下2—4h;然后自然降温到室温20—25℃;其中所述步骤1中,所述硅橡胶生胶为甲基乙烯基硅橡胶;所述步骤3中,所述氧化铁修饰碳纳米管按照下述方法进行制备:称取前驱体Fe(NO3)3·9H2O将置于无水乙醇中,加入酸化的碳纳米管,分散均匀后加入表面活性剂十二烷基苯磺酸钠,然后加入过量氨水,静置后过滤,对产物洗涤干燥后,在惰性气体保护下600℃煅烧5h,随后随炉退火至室温20—25℃即可,其中所述Fe(NO3)3·9H2O的加入量为0.5—4质量份、酸化的碳纳米管的加入量为0.35质量份、氨水的加入量为24—64质量份、表面活性剂十二烷基苯磺酸钠的加入量为0.04—0.32质量份;中国专利201410406673.7公开的一种含有碳纳米管的硅橡胶复合材料的制备方法,其特征在于,具体包括以下步骤:(1)预分散:按重量份数计,将1-10份聚倍半硅氧烷和0.1-5份碳纳米管添加到溶剂中,首先用磁力搅拌分散10-30min,然后在室温条件下,采用功率1000-500000Hz的超声分散10-30min,得到碳纳米管悬浮液;溶剂的用量为1g碳纳米管用25-50ml溶剂,所述聚倍半硅氧烷为八乙烯基聚倍半硅氧烷;(2)碳纳米管/硅橡胶原料共混物的制备:先将硅橡胶原料溶于溶剂,然后与碳纳米管悬浮液混合,并高速搅拌,条件依次为:首先500rpm搅拌5min,然后2000rpm搅拌15min,最后3000rpm搅拌15min;得到聚倍半硅氧烷/碳纳米管/硅橡胶的混合溶液,排除溶剂后,得到碳纳米管/硅橡胶原料共混物;硅橡胶原料为乙烯基封端的液体硅橡胶时,溶剂中硅橡胶原料的投料为1ml溶剂投入1g硅橡胶原料;硅橡胶原料为乙烯基封端的固体硅橡胶时,溶剂中硅橡胶原料的投料为3-5ml溶剂投入1g硅橡胶原料;(3)碳纳米管/硅橡胶共混物的成型:A硅橡胶原料为乙烯基封端的液体硅橡胶的成型将步骤(2)得到的共混物中的1/3-1/2与含氢硅油共混,其余部分与催化剂及助剂共混,然后将上述两部分料搅拌共混后脱泡,移入模具,加热硫化,制备得到硅橡胶复合材料;硫化工艺为60-150℃下硫化0.25-5h;得到含有碳纳米管的硅橡胶复合材料;B硅橡胶原料为乙烯基封端的固体硅橡胶在步骤(2)得到的共混物中添加硫化剂,在平板硫化机中经高温硫化后得到硅橡胶复合材料;硫化工艺为170-190℃、5-15Mpa下,硫化10-15min;得到含有碳纳米管的硅橡胶复合材料;乳液共混法能够使CNT等填料在橡胶基体中分散较为均匀,通常使用酸等破乳剂实现乳胶粒子和CNT的共沉淀,但是加酸或其他化学试剂絮凝及后续脱水烘干过程容易使填料发生再次团聚,造成效率低、耗时长和耗水量大的问题;同时机械共混法、溶液共混法和熔融共混法由于工艺问题,制备的橡胶复合材料也存在一些不可避免的缺陷。因此,研发设计一种GO/CNT/IIR复合材料的新型制备方法,具有良好的社会和经济价值,应用前景广阔。
发明内容:
本发明的目的在于克服现有技术存在的缺点,设计一种GO/CNT/IIR高导热复合材料制备方法,促进GO与CNT在IIRL中的分散,构建良好的导热网络,提高复合材料的导热性能。
为了实现上述目的,本发明涉及的GO/CNT/IIR高导热复合材料制备方法为干冰膨胀预分散絮凝法,其工艺过程包括制备GO/CNT/IIRL混合液、制备GO/CNT/IIRL混合液的凝固体、制备GO/CNT/IIRL母胶和制备硫化胶片共四个步骤:
(一)制备GO/CNT/IIRL混合液:将1-10phr固含量为10mg/ml的氧化石墨烯水分散液与3-6phrCNT超声处理后与质量百分比浓度为42%的丁基胶乳混合,加入20phr干冰溶解膨胀,再用叶片式搅拌器机械搅拌10min,得到分散和混合均匀的GO/CNT/IIRL混合液;
(二)制备GO/CNT/IIRL混合液的凝固体:将GO/CNT/IIRL混合液缓慢倒入絮凝剂氯化镁溶液中,进行共絮凝,GO/CNT/IIRL混合液遇到氯化镁后打破原有的电离平衡从而凝固,得到GO/CNT/IIRL混合液的凝固体;
(三)制备GO/CNT/IIR母胶:用去离子水对剪碎后的GO/CNT/IIRL混合液的凝固体冲洗,然后放压板机上压干水分,冲洗后放入温度为60℃的真空烘箱中干燥20h,得到干燥的GO/CNT/IIR母胶;
(四)制备硫化胶片:采用双辊开炼机对GO/IIR母胶进行常温开炼,依次加入2phrSAD(硬脂酸)、5phrZnO(氧化锌)、1phrRD(防老剂)、1phr防老剂4020、1phrTMTD(超促进剂)和2phrS(硫磺),薄通后下片得到混炼胶,停放24h,在温度为170℃,压力为10MPa的条件下用平板硫化剂对混炼胶进行硫化,得到硫化胶片。
本发明涉及的丁基胶乳中丁基胶的干重为100phr;絮凝剂氯化镁溶液的重量占GO/CNT/IIRL混合液的0.5-1%。
本发明与现有技术相比,基于干冰易升华的特点,将其引入到氧化石墨烯/碳纳米管/丁基胶乳的混合液中,干冰在遇热时体积瞬间能膨胀600-800倍,气泡膨胀破裂产生的极大能量,类似于微型爆炸,爆炸冲击波促使胶料分子链断裂,降低胶料的粘度,从而有利于纳米填料的分散。由于干冰升华吸收大量的热,使橡胶分子链骤冷,刚性增加,导致转子的剪切作用力更有效的传导入橡胶内部,使氧化石墨烯团聚体破碎,带动GO和CNT的分散,增大GO、CNT与IIRL中橡胶烃的接触面积,提高GO/CNT/IIR复合材料的导热性能;其工艺简单可控,原理科学合理,能耗和生产成本低,操作性强,使用环境友好,易于大规模生产和推广使用,对环保有重要的积极意义,且制备的复合材料性能和经济价值更高。
附图说明:
图1为本发明的工艺流程框图。
具体实施方式:
下面通过实施例并结合附图做进一步说明。
实施例1:
本实施例涉及的GO/CNT/IIR高导热复合材料制备方法为干冰膨胀预分散絮凝法,其工艺过程包括制备GO/CNT/IIRL混合液、制备GO/CNT/IIRL混合液的凝固体、制备GO/CNT/IIRL母胶和制备硫化胶片共四个步骤:
(一)制备GO/CNT/IIRL混合液:将3phr固含量为10mg/ml的氧化石墨烯水分散液与3phrCNT超声处理后与质量百分比浓度为42%的丁基胶乳混合,加入20phr干冰溶解膨胀,再用叶片式搅拌器机械搅拌10min,得到分散和混合均匀的GO/CNT/IIRL混合液;
(二)制备GO/CNT/IIRL混合液的凝固体:将GO/CNT/IIRL混合液缓慢倒入絮凝剂氯化镁溶液中,进行共絮凝,GO/CNT/IIRL混合液遇到氯化镁后打破原有的电离平衡从而凝固,得到GO/CNT/IIRL混合液的凝固体;
(三)制备GO/CNT/IIR母胶:用去离子水对剪碎后的GO/CNT/IIRL混合液的凝固体冲洗,然后放压板机上压干水分,冲洗后放入温度为60℃的真空烘箱中干燥20h,得到干燥的GO/CNT/IIR母胶;
(四)制备硫化胶片:采用双辊开炼机对GO/IIR母胶进行常温开炼,依次加入2phrSAD(硬脂酸)、5phrZnO(氧化锌)、1phrRD(防老剂)、1phr防老剂4020、1phrTMTD(超促进剂)和2phrS(硫磺),薄通后下片得到混炼胶,停放24h,在温度为170℃,压力为10MPa的条件下用平板硫化剂对混炼胶进行硫化,得到硫化胶片1。
实施例2:
本实施例涉及的GO/CNT/IIR高导热复合材料制备方法为干冰膨胀预分散絮凝法,其工艺过程包括制备GO/CNT/IIRL混合液、制备GO/CNT/IIRL混合液的凝固体、制备GO/CNT/IIRL母胶和制备硫化胶片共四个步骤:
(一)制备GO/CNT/IIRL混合液:将5phr固含量为10mg/ml的氧化石墨烯水分散液与5phrCNT超声处理后与质量百分比浓度为42%的丁基胶乳混合,加入20phr干冰溶解膨胀,再用叶片式搅拌器机械搅拌10min,得到分散和混合均匀的GO/CNT/IIRL混合液;
(二)制备GO/CNT/IIRL混合液的凝固体:将GO/CNT/IIRL混合液缓慢倒入絮凝剂氯化镁溶液中,进行共絮凝,GO/CNT/IIRL混合液遇到氯化镁后打破原有的电离平衡从而凝固,得到GO/CNT/IIRL混合液的凝固体;
(三)制备GO/CNT/IIR母胶:用去离子水对剪碎后的GO/CNT/IIRL混合液的凝固体冲洗,然后放压板机上压干水分,冲洗后放入温度为60℃的真空烘箱中干燥20h,得到干燥的GO/CNT/IIR母胶;
(四)制备硫化胶片:采用双辊开炼机对GO/IIR母胶进行常温开炼,依次加入2phrSAD(硬脂酸)、5phrZnO(氧化锌)、1phrRD(防老剂)、1phr防老剂4020、1phrTMTD(超促进剂)和2phrS(硫磺),薄通后下片得到混炼胶,停放24h,在温度为170℃,压力为10MPa的条件下用平板硫化剂对混炼胶进行硫化,得到硫化胶片2。
实施例3:
本实施例作为对照试验,工艺过程包括制备IIRL混合液、制备IIRL混合液的凝固体、制备IIR母胶和制备硫化胶片共四个步骤:
(一)制备IIRL混合液:称取20phr干冰溶解膨胀400g丁基胶乳,再用叶片式搅拌器机械搅拌10min,得到分散和混合均匀的IIRL混合液;
(二)制备IIRL混合液的凝固体:将IIRL混合液缓慢倒入絮凝剂氯化镁溶液中,进行共絮凝,IIRL混合液遇到氯化镁后打破原有的电离平衡从而凝固,得到IIRL混合液的凝固体;
(三)制备IIR母胶:用去离子水对剪碎后的IIRL混合液的凝固体冲洗,然后放压板机上压干水分,冲洗后放入温度为60℃的真空烘箱中干燥20h,得到干燥的IIR母胶;
(四)制备硫化胶片:采用双辊开炼机对IIR母胶进行常温开炼,依次加入2phrSAD(硬脂酸)、5phrZnO(氧化锌)、1phrRD(防老剂)、1phr防老剂4020、1phrTMTD(超促进剂)和2phrS(硫磺),薄通后下片得到混炼胶,停放24h,在温度为170℃,压力为10MPa的条件下用平板硫化剂对混炼胶进行硫化,得到硫化胶片3。
实施例4:
分别将硫化胶片1、2和3制成直径为50mm,厚度为2mm的薄片进行实验分析,采用DTC-300型导热仪分别检测硫化胶片1、2和3导热系数,检测结果显示硫化胶片1、2和3的导热系数(W/m.k)分别为0.383、0.423和0.163,表明,通过干冰的升华膨胀预分散,氧化石墨烯与CNT能够均匀的分散在丁基橡胶中,大大提高GO/CNT/IIR高导热复合材料的导热性能。
Claims (2)
1.一种GO/CNT/IIR高导热复合材料制备方法,其特征在于为干冰膨胀预分散絮凝法,其工艺过程包括制备GO/CNT/IIRL混合液、制备GO/CNT/IIRL混合液的凝固体、制备GO/CNT/IIRL母胶和制备硫化胶片共四个步骤:
(一)制备GO/CNT/IIRL混合液:将1-10phr固含量为10mg/ml的氧化石墨烯水分散液与3-6phrCNT超声处理后与质量百分比浓度为42%的丁基胶乳混合,加入20phr干冰溶解膨胀,再用叶片式搅拌器机械搅拌10min,得到分散和混合均匀的GO/CNT/IIRL混合液;
(二)制备GO/CNT/IIRL混合液的凝固体:将GO/CNT/IIRL混合液缓慢倒入絮凝剂氯化镁溶液中,进行共絮凝,GO/CNT/IIRL混合液遇到氯化镁后打破原有的电离平衡从而凝固,得到GO/CNT/IIRL混合液的凝固体;
(三)制备GO/CNT/IIR母胶:用去离子水对剪碎后的GO/CNT/IIRL混合液的凝固体冲洗,然后放压板机上压干水分,冲洗后放入温度为60℃的真空烘箱中干燥20h,得到干燥的GO/CNT/IIR母胶;
(四)制备硫化胶片:采用双辊开炼机对GO/IIR母胶进行常温开炼,依次加入2phrSAD、5phrZnO、1phrRD、1phr防老剂4020、1phrTMTD和2phrS,薄通后下片得到混炼胶,停放24h,在温度为170℃,压力为10MPa的条件下用平板硫化剂对混炼胶进行硫化,得到硫化胶片。
2.根据权利要求1所述的GO/CNT/IIR高导热复合材料制备方法,其特征在于丁基胶乳中丁基胶的干重为100phr;絮凝剂氯化镁溶液的重量占GO/CNT/IIRL混合液的0.5-1%。
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