CN110466215A - 一种改进的节能环保恒温袋及其制备方法 - Google Patents
一种改进的节能环保恒温袋及其制备方法 Download PDFInfo
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- CN110466215A CN110466215A CN201910776925.8A CN201910776925A CN110466215A CN 110466215 A CN110466215 A CN 110466215A CN 201910776925 A CN201910776925 A CN 201910776925A CN 110466215 A CN110466215 A CN 110466215A
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- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及保温材料技术领域,更具体地,本发明涉及一种改进的节能环保恒温袋。该恒温袋由二氧化硅气凝胶与橡胶发泡层两部分粘结而成,各部分均有较好的保温性能,实现“双重保温”。通过改变条件灵活调控交联网络的形成,以期达到较好的力学性能,提高恒温袋的实用性。同时,该保温袋可再循环利用,利于节能环保。
Description
技术领域
本发明涉及保温材料技术领域,更具体地,本发明涉及一种改进的节能环保恒温袋及其制备方法。
背景技术
当今世界,能源的不足以及不合理利用制约着当今人类社会进步、经济可持续发展,保温隔热材料的出现有效提高能源利用效率。因此,在新材料研究方面,开发效率高、价格低廉的保温隔热材料,对自然资源和有限能源的高效利用、节能降耗减排和经济的可持续发展具有重大的意义。
恒温袋作为一种保温隔热材料,对其保温效果及使用方面提出严格要求,但是目前所使用的恒温袋保温效果差,或者需要通过填加大量保温材料来达到较好的保温效果,造成材料浪费的同时限制了恒温袋的力学性能(弹性模量),因此,本发明致力于制备一种改进的节能环保恒温袋。
发明内容
为了解决上述问题,本发明第一方面提供了一种改进的节能环保恒温袋,该节能环保恒温袋由二氧化硅气凝胶与橡胶发泡层组成,其中,按重量份计,橡胶发泡层包括:基体55~85份、硫化体系3~15份、助剂5~25份。
作为本发明的一种优选技术方案,其中,所述二氧化硅气凝胶的制备方法为:
a.将环氧基硅烷、氨基烯类化合物加入醇钠溶液中,于60~90℃反应7~10h,将环氧基硅烷与氨基烯类化合物反应后产物与溶剂混合,调节pH使其溶胶-凝胶化,并移入自由基引发剂溶液中,在50~80℃下引发聚合,得到中间体1;
b.将中间体1用老化剂浸泡洗涤,得到中间体2;
c.将中间体2加入硅烷化试剂溶液中静置、冲洗,最后在60~100℃条件下干燥,得到二氧化硅气凝胶。
作为本发明的一种优选技术方案,其中,所述环氧基硅烷的结构为 中任一种或多种组合,其中R1、R2、R4、R5独立选自甲基、甲氧基、乙氧基中任一种,R3、R6各含有环氧基团。
作为本发明的一种优选技术方案,其中,所述环氧基硅烷包括二乙氧基甲基[(3-环氧乙烷基甲氧)丙基]硅烷、3-缩水甘油醚氧基丙基三乙氧基硅烷、3-缩水甘油醚氧基丙基三甲氧基硅烷、(3-环氧丙氧基丙基)二甲基乙氧基硅烷、3-[(2,3)-环氧丙氧]丙基甲基二甲氧基硅烷。
作为本发明的一种优选技术方案,其中,所述氨基烯类化合物包括3-丁烯-1-胺、4-戊烯-1-胺、(E)-丁-2-烯-1-胺、3-甲基-2-丁烯胺、1-氨基-5-己烯。
作为本发明的一种优选技术方案,其中,所述环氧基硅烷、氨基烯类化合物的摩尔比为1:(0.5~1.3)。
作为本发明的一种优选技术方案,其中,所述硫化体系包括硫化剂、促进剂、活性剂、防焦剂。
作为本发明的一种优选技术方案,其中,所述硫化剂、促进剂、活性剂、防焦剂摩尔比依次为1:(1~1.5):(0.2~0.7):(0.2~0.7)。
作为本发明的一种优选技术方案,其中,所述硫化剂为改性高岭土硫化剂。
本发明第二方面提供了改进的节能环保恒温袋制备方法,其中,所述二氧化硅气凝胶表面涂覆胶黏剂,后将二氧化硅气凝胶粘层与橡胶发泡层粘合制备节能环保恒温袋。
有益效果
利用本发明制备的节能环保恒温袋具有较好的保温性能与实用性,具体表现为该恒温袋由二氧化硅气凝胶与橡胶发泡层两部分粘结而成,实现“双重保温”;通过改变条件灵活调控交联网络的形成,以期达到较好的力学性能,尤其是弹性模量,提高恒温袋的实用性;可再循环利用,利于节能环保。
具体实施方式
下面结合具体实施方式对本发明提供技术方案中的技术特征作进一步清楚、完整的描述,并非对其保护范围的限制。
本发明中的词语“优选的”、“更优选的”等是指,在某些情况下可提供某些有益效果的本发明实施方案。然而,在相同的情况下或其他情况下,其他实施方案也可能是优选的。此外,对一个或多个优选实施方案的表述并不暗示其他实施方案不可用,也并非旨在将其他实施方案排除在本发明的范围之外。
本发明第一方面提供了一种改进的节能环保恒温袋,该节能环保恒温袋由二氧化硅气凝胶与橡胶发泡层组成,其中,按重量份计,橡胶发泡层包括:基体55~85份、硫化体系3~15份、助剂5~25份。
二氧化硅气凝胶
气凝胶通常是指以纳米量级超微颗粒相互聚集构成纳米多孔网络结构,并在网络孔隙中充满气态分散介质的轻质纳米固体材料。气凝胶是一种固体,但是99%都是由气体构成,因其半透明的色彩和超轻重量,气凝胶也被称为“固态烟”或“冻住的烟”。因其特殊的纳米多孔网络结构,气凝胶材料具有高孔隙率、高表面活性、高比表面积、低密度、低热导率等特殊性质,在很多领域都有着非常广阔的应用前景。
在一种优选的实施方式中,所述二氧化硅气凝胶的制备方法如下:
a.将环氧基硅烷、氨基烯类化合物加入醇钠溶液中,于60~90℃反应7~10h,将环氧基硅烷与氨基烯类化合物反应后产物与溶剂混合,调节pH使其溶胶-凝胶化,并移入自由基引发剂溶液中,在50~80℃下引发聚合,得到中间体1;
b.将中间体1用老化剂浸泡洗涤,得到中间体2;
c.将中间体2加入硅烷化试剂溶液中静置、冲洗,最后在60~100℃条件下干燥,得到二氧化硅气凝胶。
在一种优选的实施方式中,所述环氧基硅烷、氨基烯类化合物的摩尔比为1:(0.5~1.3)。
更优选地,所述环氧基硅烷、氨基烯类化合物的摩尔比为1:1。
在一种优选的实施方式中,所述醇钠溶液的浓度为2.5g/L。
(环氧基硅烷)
在一种优选的实施方式中,所述环氧基硅烷的结构为 中任一种或多种组合,其中R1、R2、R4、R5独立选自甲基、甲氧基、乙氧基中任一种,R3、R6各含有环氧基团。
作为环氧基硅烷的实例,包括但不限于:环氧基硅烷选自二乙氧基甲基[(3-环氧乙烷基甲氧)丙基]硅烷、3-缩水甘油醚氧基丙基三乙氧基硅烷、3-缩水甘油醚氧基丙基三甲氧基硅烷、(3-环氧丙氧基丙基)二甲基乙氧基硅烷、3-[(2,3)-环氧丙氧]丙基甲基二甲氧基硅烷中任一种或多种的组合。
更优选地,所述环氧基硅烷为二乙氧基甲基[(3-环氧乙烷基甲氧)丙基]硅烷(CAS:2897-60-1)。
(氨基烯类化合物)
在一种优选的实施方式中,所述氨基烯类化合物包括但不限于:3-丁烯-1-胺、4-戊烯-1-胺、(E)-丁-2-烯-1-胺、3-甲基-2-丁烯胺、1-氨基-5-己烯中任一种或多种的组合。
更优选地,所述氨基烯类化合物为3-丁烯-1-胺(CAS:2524-49-4)。
在一种优选的实施方式中,所述调节pH为稀盐酸先将体系调至pH=1~5,5h后用氨水调至pH=6~8。
[溶胶-凝胶化]
溶胶-凝胶化(Sol-Gel法,简称S-G法)就是以金属醇盐或无机物作前驱体,在液相将这些原料均匀混合,并进行水解、缩合化学反应,在溶液中形成稳定的透明溶胶体系,溶胶经陈化后胶粒间缓慢聚合,形成三维空间网络结构的凝胶。
[自由基引发剂]
自由基引发剂指一类容易受热分解成自由基(即初级自由基)的化合物,可用于引发烯类、双烯类单体的自由基聚合或共聚合反应,也可用于不饱和聚酯的交联固化和高分子交联反应。
在一种优选的实施方式中,所述自由基引发剂选自有机过氧化物引发剂(过氧化苯甲酰、叔丁基过氧化氢、过氧化环己酮等),无机过氧化物引发剂(过硫酸铵、过硫酸钾等),偶氮类引发剂(偶氮二异丁腈、偶氮二异庚腈等),氧化还原引发剂(过氧化苯甲酰/N,N-二甲基苯胺、过硫酸铵/亚硫酸氢钠等)中任一种或多种的组合。
更优选地,所述自由基引发剂为偶氮二异丁腈(CAS:78-67-1)。
[老化剂]
在一种优选的实施方式中,所述老化剂选自甲醇、乙醇、异丙醇、丙酮、正己烷、正庚烷中任一种或多种的组合。
更优选地,所述老化剂为正己烷(CAS:110-54-3)。
[硅烷化试剂]
硅烷化试剂简写SBA,又称硅烷保护剂。在分析或有机合成中用以变更或保护有机物中活性基团的一类有机硅单体或小分子化合物。硅烷化试剂有五十余种,主要包括:
(1)三甲基甲硅烷基单官能SBA,如三甲基氯硅烷(TMCS)、六甲基二硅氮烷(HMDZ)等;
(2)位阻型单官能SBA,如叔丁基二甲基氯硅烷(TBSCI)、三异丙基氧硅烷等;
(3)位阻型双官能SBA,如二甲基二乙酰氧基硅烷、二叔丁基二氯硅烷等;
(4)其它硅烷化试剂,如三甲基轻乙基硅烷、甲基二苯基羟乙基硅烷等。在一种优选的实施方式中,所述硅烷化试剂选自三甲基氯硅烷(TMCS)、六甲基二硅烷(HMDS)、六甲基二硅氮烷(HMDZ)、六甲基二硅氧烷(HMDSO)、三甲基乙氧基硅烷(MTES)、甲基三甲氧基硅烷(MTMS)、乙烯基三甲氧基硅烷(A-171系硅烷偶联剂)、苯基三甲氧基硅烷、苯基三乙氧基硅烷、二甲基二甲氧基硅烷、三甲基甲氧基硅烷中任一种或多种的组合。
更优选地,所述硅烷化试剂为三甲基氯硅烷(CAS:75-77-4)。
在一种优选的实施方式中,所述硅烷化试剂与正己烷的体积比为1:(5~15)。
更优选地,所述硅烷化试剂与正己烷的体积比为1:10。
本发明人发现SiO2气凝胶具有良好的保温性能,但是当气凝胶受到外力作用时,导致SiO2气凝胶脆性大,限制SiO2气凝胶的实用性。本发明制备的SiO2气凝胶除Si-O-Si构成的交联链外,同时引入了大量的柔性链(C-O,C-N,C-C键),当其受到外力作用时,该柔性链可以使部分应力分散,从而保护SiO2气凝胶粒子间的连接部分。同时,本发明人意外发现,当所述环氧基硅烷为二乙氧基甲基[(3-环氧乙烷基甲氧)丙基]硅烷、氨基烯类化合物为3-丁烯-1-胺时,SiO2气凝胶的韧性和强度都得到提高,发明人推测可能的原因是:随着CH3/Si比的增加,可更多的增加柔性链的相对数量,减少刚性链,并且柔性链长度适宜;同时由于基团与基团之间的作用,限制了Si-O-Si链接个数,但是通过双键或环氧开环反应获得柔性链并使之整个结构连接,从而整体刚柔“并济”。与此同时,Si-O-Si、双键、-NH2基团等相互作用,也促使气凝胶孔结构的“曲折性”,提高了保温效果。
橡胶发泡层
橡胶发泡是指用特定的发泡剂处理橡胶从而使橡胶具有特征性能的处理手段,在橡胶发泡层中气体和橡胶固体共存。在性质上,气体与橡胶固体存在巨大差异,橡胶发泡层中的气体对材料的结构、形态和性能均存在较大的影响。橡胶发泡层是通过橡胶和泡孔内的气体进行传热的,由于泡孔中气体占据材料大量的体积,因而泡内气体是主要的导热介质,而气体的热导率很低,从而使得橡胶发泡具有较低的热导率,同时泡孔壁能使泡孔间的对流传热大幅削减,能提高保温性能。
在一种优选的实施方式中,按重量份计,所述橡胶发泡层包括:基体55~85份、硫化体系3~15份、助剂5~25份。
更优选地,所述橡胶发泡层包括:基体70份、硫化体系10份、助剂20份。
在一种优选的实施方式中,所述基体选自天然橡胶、丁苯橡胶、顺丁橡胶中任一种或多种的组合。
更优选地,所述基体为天然橡胶与丁苯橡胶混合物。
更优选地,天然橡胶与丁苯橡胶质量份比为1:1。
在一种优选的实施方式中,所述硫化体系包括硫化剂、促进剂、活性剂、防焦剂。
在一种优选的实施方式中,所述硫化剂、促进剂、活性剂、防焦剂摩尔比为1:(1~1.5):(0.2~0.7):(0.2~0.7)。
更优选地,所述硫化剂、促进剂、活性剂、防焦剂摩尔比为1:1.2:0.3:0.2。[硫化剂]
硫化剂能在一定条件下使橡胶发生硫化的物质统称为硫化剂,所谓硫化是使橡胶线性分子结构通过硫化剂的“架桥”而变成立体网状机构,从而使橡胶的机械物理性能得到明显的改善。
在一种优选的实施方式中,所述硫化剂选自元素硫、硒、碲、含硫化合物、过氧化物、醌类化合物、胺类化合物、树脂类化合物、金属氧化物以及异氰酸酯中任一种或多种的组合。
更优选地,所述硫化剂为改性高岭土硫化剂。
在一种优选的实施方式中,所述改性高岭土硫化剂的制备方法如下:
(1)在20~50℃条件下,将高岭土在丙烯酰胺水溶液中搅拌2~5h后过滤,150~200℃条件下烘干后得到酰胺改性高岭土;
(2)将酰胺改性高岭土分散在二乙醚溶剂中,搅拌过程中滴加氯化硫(S2Cl2),并在20~45℃氮气保护下反应5~10h,用无水乙醇洗涤后真空干燥得到改性高岭土硫化剂。
高岭土是一种非金属矿产,是一种以高岭石族粘土矿物为主的粘土和粘土岩。其质纯的高岭土呈洁白细腻、松软土状,具有良好的可塑性和耐火性等理化性质。其矿物成分主要由高岭石、埃洛石、水云母、伊利石、蒙脱石以及石英、长石等矿物组成。高岭土用途十分广泛,主要用于造纸、陶瓷和耐火材料,其次用于涂料、橡胶填料、搪瓷釉料和白水泥原料,少量用于塑料、油漆、颜料、砂轮、铅笔、日用化妆品、肥皂、农药、医药、纺织、石油、化工、建材、国防等工业部门。
粒度是指颗粒的大小。通常球体颗粒的粒度用直径表示,立方体颗粒的粒度用边长表示。对不规则的颗粒,可将与该颗粒有相同行为的某一球体直径作为该颗粒的等效直径。
在一种优选的实施方式中,所述改性高岭土硫化剂中高岭土粒度为0.3~1μm,可以通过商购得到,例如可商购得到的高岭土包括但不限于购买自巴斯夫公司。
更优选地,所述改性高岭土硫化剂中高岭土粒度为0.5μm。
在一种优选的实施方式中,所述丙烯酰胺水溶液质量浓度为5~25wt%。
更优选地,所述丙烯酰胺水溶液的质量浓度为10wt%。
在一种优选的实施方式中,所述高岭土与丙烯酰胺的质量份比为1:(0.1~0.5)。
更优选地,所述高岭土与丙烯酰胺的质量份比为1:0.3。
在一种优选的实施方式中,所述酰胺改性高岭土与S2Cl2的质量份比为1:(0.5~0.9)。
更优选地,所述酰胺改性高岭土与S2Cl2的质量份比为1:0.7。
[促进剂]
促进剂缩短橡胶的硫化时间或降低硫化温度,减少硫化剂用量及提高橡胶的物理机械性能等。
在一种优选的实施方式中,所述促进剂选自醛胺类(如硫化促进剂H)、胍类(如硫化促进剂D)、秋兰姆类(如硫化促进剂TMTD)、噻唑类(如硫化促进剂M)、二硫代氨基甲酸盐类(如硫化促进剂ZDMC)、黄原酸盐类(如硫化促进剂ZBX)、硫脲类(如硫化促进剂NA-22)、次磺酰胺类(如硫化促进剂CZ)中任一种或多种的组合。
更优选地,所述促进剂为二硫化四甲基秋兰姆(TMTD,CAS:137-26-8)。
[活性剂]
活性剂指配入胶料中后能增加促进剂活性,进而减少促进剂用量或缩短硫化时间的物质,有时也称促进助剂。加入少量活性剂能大大提高硫化胶的硫化度和耐热性。
在一种优选的实施方式中,所述活性剂选自金属氧化物(如氧化锌、活性氧化锌)、硬脂酸中任一种或多种的组合。
更优选地,所述活化剂为氧化锌和硬脂酸(CAS:4813-57-4)。
更优选地,所述氧化锌与硬脂酸的质量份比为3:1。
[防焦剂]
防焦剂是防止橡胶胶料在加工过程中产生早期硫化现象的物质。
在一种优选的实施方式中,所述防焦剂选自亚硝基化合物(如N-亚硝基二苯胺等)、有机酸类(如苯甲酸、邻苯二甲酸酐等)和硫代亚酰胺类(如N-环已基硫代邻苯二甲酰亚胺等)。常用的有草酸、琥珀酸、乳酸、邻苯二甲酸酐、水杨酸、苯甲酸、油酸中任一种或多种的组合。
更优选地,所述防焦剂为水杨酸(CAS:69-72-7)。
在一种优选的实施方式中,所述助剂包括填充剂、增塑剂、发泡剂、防老剂。
[填充剂]
填充剂加入物料中可以改善物料性能,或能增容、增重,降低物料的成本的固体物质。通常不含水、中性、不与物料组分起不良作用的有机物、无机物、金属或非金属粉末等均可作为填充剂。
在一种优选的实施方式中,所述填充剂选自硅藻土、滑石粉、石墨、可分散炭黑、氧化铝粉、玻璃粉、石棉粉、云母粉、石英粉、碳纤维、粉末状软木、金刚砂中任一种或多种的组合。
更优选地,所述填充剂为可分散炭黑(CAS:1333-86-4)。
[增塑剂]
增塑剂分布在大分子链之间,能降低分子间作用力,使聚合物粘度降低,柔韧性增强,普遍应用于塑料制品、混凝土、泥灰、水泥、石膏、化妆品及清洗剂等材料中。
在一种优选的实施方式中,所述增塑剂选自古马隆树脂、邻苯二甲酸酯、脂肪族二元酸酯、脂肪酸酯、苯多酸酯、多元醇酯、环氧烃类、烷基磺酸酯中任一种或多种的组合。
更优选地,所述增塑剂为古马隆树脂(CAS:63393-89-5)。
[发泡剂]
发泡剂就是使对象物质成孔的物质,它可分为化学发泡剂、物理发泡剂两大类。化学发泡剂是经加热分解后能释放出二氧化碳和氮气等气体,并在聚合物组成中形成细孔的化合物;物理发泡剂就是泡沫细孔是通过某一种物质的物理形态的变化,即通过压缩气体的膨胀、液体的挥发或固体的溶解而形成的。发泡剂均具有较高的表面活性,能有效降低液体的表面张力,并在液膜表面双电子层排列而包围空气,形成气泡,再由单个气泡组成泡沫。
在一种优选的实施方式中,所述发泡剂选自碳酸氢钠、碳酸氢铵、偶氮二甲酰胺、二苯磺酰肼醚、二偶氮氨基苯、对甲苯磺酰肼、N,N-二亚硝基五次甲基四胺中任一种或多种的组合。
更优选地,所述发泡剂为碳酸氢钠(CAS:144-55-8)。
[防老剂]
防老剂用以抵抗橡胶及其制品在长期贮存和使用过程中受到热、氧、臭氧等破坏作用,延缓或抑制老化过程,从而延长橡胶及其制品的贮存期和使用寿命。
在一种优选的实施方式中,所述防老剂选自胺类防老剂(酮胺、N-苯基-α-苯胺、N-苯基-β-萘胺等)、对苯二胺类防老剂(N-苯基-N'-异丙基-对苯二胺、N-N'-二苯基-对苯二胺等)、酚类防老剂、杂环类防老剂中任一种或多种的组合。
更优选地,所述防老剂为N-苯基-β-萘胺(CAS:135-88-6)。
在一种优选的实施方式中,所述橡胶发泡层的制备方法如下:
(1)将基体在开炼机上薄通三次;
(2)依次加入填充剂、增塑剂、发泡剂、防老剂、防焦剂、活性剂、促进剂及高岭土硫化剂载体并混炼均匀,在120~200℃条件下混炼10~30min,制备橡胶发泡层。
在一种优选的实施方式中,所述填充剂、增塑剂、发泡剂、防老剂的质量份比为(3~6):(3~6):(1.5~2.5):(1~2)。
更优选地,所述填充剂、增塑剂、发泡剂、防老剂的质量份比为5:5:2:1.5。
本发明人发现高岭土在橡胶基体中分散性较差主要有两方面原因:1.粒度影响,当高岭土粒度为0.3~1μm时才能更好的分散在橡胶集体中,有补强与填充两方面作用;2.由于其特殊的片层结构导致其在橡胶基体中的分散性较差,极性小分子丙烯酰胺可直接进行高岭土的插层反应,增大高岭土层间距,并增强高岭土的有机相容性。高岭土作为一种负硫载体,可随硫化温度的升高分解出活性硫进行硫化反应,得到硫化效果较好的橡胶发泡材料。同时发明人意外发现,当加入极性小分子丙烯酰胺时,提高了塑料袋的力学性能,发明人推测可能的原因是:改性高岭土中的活性基团与氯化硫相互作用,一方面提高了载硫量,另一方面提高改性高岭土与体系的相容性;同时改性后高岭土中的含硫物质在硫化过程中依据硫化温度的不同,依次分解得到活性硫,从而提高了塑料袋的力学性能。
本发明第二个方面提供了改进节能环保恒温袋的制备方法,二氧化硅气凝胶表面涂覆胶黏剂,后将二氧化硅气凝胶粘层与橡胶发泡层粘合制备节能环保恒温袋。
更优选地,所述胶黏剂为环氧树脂胶黏剂。
更优选地,环氧树脂胶黏剂与二氧化硅气凝胶的质量比为1:20。
在一种优选的实施方式中,所述二氧化硅气凝胶的厚度为1~2mm。
更优选地,所述二氧化硅气凝胶的厚度为1.5mm。
更优选地,二氧化硅气凝胶与橡胶发泡层的厚度比为1:1。
实施例1
本发明的实施例1提供了一种改进的节能环保恒温袋,其中,按重量份计,橡胶发泡层包括55份基体、3份硫化体系、5份助剂。
所述二氧化硅气凝胶的制备方法如下:
(a)将1g环氧基硅烷与0.14g氨基烯类化合物分别加入200mL甲醇钠-甲醇溶液中,于70℃反应8h,将环氧基硅烷与氨基烯类化合物反应后处理产物加入烧杯中,并加入250mL乙醇作为溶剂,混合均匀后,加入0.1mol/L草酸调节pH=3,磁力搅拌60min后用0.5mol/L氨水调节pH=7,搅拌均匀后静置5h使其溶胶-凝胶化,加入0.05g自由基引发剂,在70℃下引发聚合,得到中间体1;
(b)将中间体1用老化剂浸泡洗涤,得到中间体2;
(c)将中间体2加入200mL硅烷化试剂-正己烷混合溶液中静置,之后用正己烷冲洗,最后在80℃条件下干燥,得到二氧化硅气凝胶。
步骤(a)中所述环氧基硅烷为二乙氧基甲基[(3-环氧乙烷基甲氧)丙基]硅烷;
步骤(a)中所述氨基烯类化合物为3-丁烯-1-胺;
步骤(a)中所述甲醇钠-甲醇溶液的浓度为2.5g/L;
步骤(a)中自由基引发剂为偶氮二异丁腈;
步骤(b)中所述老化剂为正己烷;
步骤(c)中所述硅烷化试剂为三甲基氯硅烷(TMCS);
步骤(c)中所述硅烷化试剂与正己烷的体积比为1:10;
所述基体为天然橡胶与丁苯橡胶混合物;
所述天然橡胶与丁苯橡胶的质量份比为1:1;
所述硫化体系包括硫化剂、促进剂、活性剂、防焦剂;
所述硫化剂为改性高岭土硫化剂;
所述改性高岭土硫化剂中高岭土粒度为0.5μm;
所述促进剂为TMTD;
所述活性剂为氧化锌和硬脂酸;
所述氧化锌与硬脂酸的质量份比为3:1;
所述防焦剂为水杨酸;
所述硫化剂、促进剂、活性剂、防焦剂的摩尔比为1:1.2:0.3:0.2;
所述改性高岭土的制备方法如下:
(1)在30℃条件下,将2g高岭土在丙烯酰胺水溶液中搅拌4h后过滤,170℃条件下烘干后得到酰胺改性高岭土;
(2)将酰胺改性高岭土分散在250mL二乙醚溶剂中,搅拌过程中滴加氯化硫(S2Cl2),并在30℃氮气保护下反应7h,用无水乙醇洗涤后真空干燥得到改性高岭土硫化剂。
步骤(1)所述丙烯酰胺水溶液质量浓度为10wt%;
步骤(1)所述高岭土与丙烯酰胺的质量份比为1:0.3;
步骤(2)所述酰胺改性高岭土与S2Cl2的质量份比为1:0.7;
所述助剂为填充剂、增塑剂、发泡剂、防老剂;
所述填充剂为可分散炭黑;
所述增塑剂为古马隆树脂;
所述发泡剂为碳酸氢钠;
所述防老剂为N-苯基-β-萘胺;
所述填充剂、增塑剂、发泡剂、防老剂的质量份比为5:5:2:1.5;
所述橡胶发泡层的制备方法如下:
(Ⅰ)将基体在开炼机上薄通三次;
(Ⅱ)依次加入填充剂、增塑剂、发泡剂、防老剂、防焦剂、活性剂、促进剂及高岭土硫化剂载体并混炼均匀,在160℃条件下混炼20min,制备橡胶发泡层。
所述节能环保恒温袋的制备方法如下:
(A)胶黏剂涂覆于二氧化硅气凝胶表面;
(B)将二氧化硅气凝胶粘层与橡胶发泡层粘合制备节能环保恒温袋。
所述胶黏剂为环氧树脂胶黏剂;
所述环氧树脂胶黏剂与二氧化硅气凝胶的质量比为1:20;
所述二氧化硅气凝胶的厚度为1.5mm;
所述二氧化硅气凝胶与橡胶发泡层的厚度比为1:1。
实施例2
本发明的实施例2提供了一种改进的节能环保恒温袋,其中,按重量份计,橡胶发泡层包括85份基体、15份硫化体系、25份助剂。
所述二氧化硅气凝胶的制备方法如下:
(a)将1g环氧基硅烷与0.37g氨基烯类化合物分别加入200mL甲醇钠-甲醇溶液中,于70℃反应8h,将环氧基硅烷与氨基烯类化合物反应后处理产物加入烧杯中,并加入250mL乙醇作为溶剂,混合均匀后,加入0.1mol/L草酸调节pH=3,磁力搅拌60min后用0.5mol/L氨水调节pH=7,搅拌均匀后静置5h使其溶胶-凝胶化,加入0.05g自由基引发剂,在70℃下引发聚合,得到中间体1;
(b)将中间体1用老化剂浸泡洗涤,得到中间体2;
(c)将中间体2加入200mL硅烷化试剂-正己烷混合溶液中静置,之后用正己烷冲洗,最后在80℃条件下干燥,得到二氧化硅气凝胶。步骤(a)中所述环氧基硅烷为二乙氧基甲基[(3-环氧乙烷基甲氧)丙基]硅烷;步骤(a)中所述氨基烯类化合物为3-丁烯-1-胺;
步骤(a)中所述甲醇钠-甲醇溶液的浓度为2.5g/L;
步骤(a)中自由基引发剂为偶氮二异丁腈;
步骤(b)中所述老化剂为正己烷;
步骤(c)中所述硅烷化试剂为三甲基氯硅烷(TMCS);
步骤(c)中所述硅烷化试剂与正己烷的体积比为1:10;
所述基体为天然橡胶与丁苯橡胶混合物;
所述天然橡胶与丁苯橡胶的质量份比为1:1;
所述硫化体系包括硫化剂、促进剂、活性剂、防焦剂;
所述硫化剂为改性高岭土硫化剂;
所述改性高岭土硫化剂中高岭土粒度为0.5μm;
所述促进剂为TMTD;
所述活性剂为氧化锌和硬脂酸;
所述氧化锌与硬脂酸的质量份比为3:1;
所述防焦剂为水杨酸;
所述硫化剂、促进剂、活性剂、防焦剂的摩尔比为1:1.2:0.3:0.2;
所述改性高岭土的制备方法如下:
(1)在30℃条件下,将2g高岭土在丙烯酰胺水溶液中搅拌4h后过滤,170℃条件下烘干后得到酰胺改性高岭土;
(2)将酰胺改性高岭土分散在250mL二乙醚溶剂中,搅拌过程中滴加氯化硫(S2Cl2),并在30℃氮气保护下反应7h,用无水乙醇洗涤后真空干燥得到改性高岭土硫化剂。
步骤(1)所述丙烯酰胺水溶液质量浓度为10wt%;
步骤(1)所述高岭土与丙烯酰胺的质量份比为1:0.3;
步骤(2)所述酰胺改性高岭土与S2Cl2的质量份比为1:0.7;
所述助剂为填充剂、增塑剂、发泡剂、防老剂;
所述填充剂为可分散炭黑;
所述增塑剂为古马隆树脂;
所述发泡剂为碳酸氢钠;
所述防老剂为N-苯基-β-萘胺;
所述填充剂、增塑剂、发泡剂、防老剂的质量份比为5:5:2:1.5;
所述橡胶发泡层的制备方法如下:
(Ⅰ)将基体在开炼机上薄通三次;
(Ⅱ)依次加入填充剂、增塑剂、发泡剂、防老剂、防焦剂、活性剂、促进剂及高岭土硫化剂载体并混炼均匀,在160℃条件下混炼20min,制备橡胶发泡层材料。
所述节能环保恒温袋的制备方法如下:
(A)胶黏剂涂覆于二氧化硅气凝胶表面;
(B)将二氧化硅气凝胶粘层与橡胶发泡层粘合制备节能环保恒温袋。
所述胶黏剂为环氧树脂胶黏剂;
所述环氧树脂胶黏剂与二氧化硅气凝胶的质量比为1:20;
所述二氧化硅气凝胶的厚度为1.5mm;
所述二氧化硅气凝胶与橡胶发泡层的厚度比为1:1。
实施例3
本发明的实施例3提供了一种改进的节能环保恒温袋,其中,按重量份计,橡胶发泡层包括70份基体、10份硫化体系、20份助剂。
所述二氧化硅气凝胶的制备方法如下:
(a)将1g环氧基硅烷与0.29g氨基烯类化合物分别加入200mL甲醇钠-甲醇溶液中,于70℃反应8h,将环氧基硅烷与氨基烯类化合物反应后处理产物加入烧杯中,并加入250mL乙醇作为溶剂,混合均匀后,加入0.1mol/L草酸调节pH=3,磁力搅拌60min后用0.5mol/L氨水调节pH=7,搅拌均匀后静置5h使其溶胶-凝胶化,加入0.05g自由基引发剂,在70℃下引发聚合,得到中间体1;
(b)将中间体1用老化剂浸泡洗涤,得到中间体2;
(c)将中间体2加入200mL硅烷化试剂-正己烷混合溶液中静置,之后用正己烷冲洗,最后在80℃条件下干燥,得到二氧化硅气凝胶。
步骤(a)中所述环氧基硅烷为二乙氧基甲基[(3-环氧乙烷基甲氧)丙基]硅烷;
步骤(a)中所述氨基烯类化合物为3-丁烯-1-胺;
步骤(a)中所述甲醇钠-甲醇溶液的浓度为2.5g/L;
步骤(a)中自由基引发剂为偶氮二异丁腈;
步骤(b)中所述老化剂为正己烷;
步骤(c)中所述硅烷化试剂为三甲基氯硅烷(TMCS);
步骤(c)中所述硅烷化试剂与正己烷的体积比为1:10;
所述基体为天然橡胶与丁苯橡胶混合物;
所述天然橡胶与丁苯橡胶的质量比为1:1;
所述硫化体系包括硫化剂、促进剂、活性剂、防焦剂;
所述硫化剂为改性高岭土硫化剂;
所述改性高岭土硫化剂中高岭土粒度为0.5μm;
所述促进剂为TMTD;
所述活性剂为氧化锌和硬脂酸;
所述氧化锌与硬脂酸的质量份比为3:1;
所述防焦剂为水杨酸;
所述硫化剂、促进剂、活性剂、防焦剂的摩尔比为1:1.2:0.3:0.2;
所述改性高岭土的制备方法如下:
(1)在30℃条件下,将2g高岭土在丙烯酰胺水溶液中搅拌4h后过滤,170℃条件下烘干后得到酰胺改性高岭土;
(2)将酰胺改性高岭土分散在250mL二乙醚溶剂中,搅拌过程中滴加氯化硫(S2Cl2),并在30℃氮气保护下反应7h,用无水乙醇洗涤后真空干燥得到改性高岭土硫化剂。
步骤(1)所述丙烯酰胺水溶液质量浓度为10wt%;
步骤(1)所述高岭土与丙烯酰胺的质量份比为1:0.3;
步骤(2)所述酰胺改性高岭土与S2Cl2的质量份比为1:0.7;
所述助剂为填充剂、增塑剂、发泡剂、防老剂;
所述填充剂为可分散炭黑;
所述增塑剂为古马隆树脂;
所述发泡剂为碳酸氢钠;
所述防老剂为N-苯基-β-萘胺;
所述填充剂、增塑剂、发泡剂、防老剂的质量份比为5:5:2:1.5;
所述橡胶发泡层的制备方法如下:
(Ⅰ)将基体在开炼机上薄通三次;
(Ⅱ)依次加入填充剂、增塑剂、发泡剂、防老剂、防焦剂、活性剂、促进剂及高岭土硫化剂载体并混炼均匀,在160℃条件下混炼20min,制备橡胶发泡层材料。
所述节能环保恒温袋的制备方法如下:
(A)胶黏剂涂覆于二氧化硅气凝胶表面;
(B)将二氧化硅气凝胶粘层与橡胶发泡层粘合制备节能环保恒温袋。
所述胶黏剂为环氧树脂胶黏剂;
所述环氧树脂胶黏剂与二氧化硅气凝胶的质量比为1:20;
所述二氧化硅气凝胶的厚度为1.5mm;
所述二氧化硅气凝胶与橡胶发泡层的厚度比为1:1。
实施例4
本发明的实施例4提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述丙烯酰胺替换为二甲亚砜。
实施例5
本发明的实施例5提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述改性高岭土硫化剂替换为高岭土和S2Cl2的混合物,其中高岭土与S2Cl2的质量份比为1:0.7。
实施例6
本发明的实施例6提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述酰胺改性高岭土与S2Cl2的质量份比为1:1.5。
实施例7
本发明的实施例7提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述酰胺改性高岭土与S2Cl2的质量份比为1:0.2。
实施例8
本发明的实施例8提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述硫化体系组分中改性高岭土硫化剂替换为硫磺。
实施例9
本发明的实施例9提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述环氧基硅烷与氨基烯类化合物的摩尔比为1:0。
实施例10
本发明的实施例10提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述环氧基硅烷与氨基烯类化合物的摩尔比为1:2。
实施例11
本发明的实施例11提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述环氧基硅烷与氨基烯类化合物的摩尔比为1:0.1。
实施例12
本发明的实施例12提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述3-丁烯-1-胺替换为1-氨基-10-十一烯。
实施例13
本发明的实施例13提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述二乙氧基甲基[(3-环氧乙烷基甲氧)丙基]硅烷替换为四乙氧基硅烷。
实施例14
本发明的实施例14提供了一种改进的节能环保恒温袋,其具体实施方式同实施例3,不同之处在于,所述二乙氧基甲基[(3-环氧乙烷基甲氧)丙基]硅烷替换为二乙氧基二甲基硅烷。
性能评价
节能环保恒温袋裁剪成10×10cm的正方形进行性能测试。
(1)热导率分析
样品热导率分为两部分测量:使用差示扫描量热仪(DSC 204HP)测量得到样品的定压比热容;使用激光闪射热分析仪(LFA457)测量得到热扩散系数,并在机器内通过计算得到热导率。定压比热容测量条件为:升温速率为10℃/min,温度范围为40~200℃,吹扫气为N2,流速为30mL/min。热扩散系数测量条件为:放大器增益为127,激光电压为1538V,采样时间为40000ms,升温速率为1℃/min,每个温度点采样数为5个,吹扫气为N2,流速为15mL/min。
(1)弹性模量分析
通过测试样品的压缩模量来描述弹性模量。将不同重量的砝码放置于样品上,计算样品所受压力,测量施加压力前后样品厚度的变化,以下公式进行计算弹性模量:
其中G为弹性模量,F为施加的力,A为受力面积,△L为厚度变化,Lo为未施加前的厚度。
实施例 | 热导率(mW/m.K) | 弹性模量(MPa) |
实施例1 | 65 | 14 |
实施例2 | 61 | 20 |
实施例3 | 40 | 16 |
实施例4 | 70 | 22 |
实施例5 | 69 | 25 |
实施例6 | 80 | 30 |
实施例7 | 85 | 18 |
实施例8 | 77 | 17 |
实施例9 | 90 | 21 |
实施例10 | 85 | 22 |
实施例11 | 78 | 20 |
实施例12 | 75 | 19 |
实施例13 | 80 | 19 |
实施例14 | 76 | 22 |
Claims (10)
1.一种改进的节能环保恒温袋,其特征在于,该节能环保恒温袋由二氧化硅气凝胶与橡胶发泡层组成,按重量份计,橡胶发泡层包括:基体55~85份、硫化体系3~15份、助剂5~25份。
2.根据权利要求1所述改进的节能环保恒温袋,其特征在于,所述二氧化硅气凝胶的制备方法为:
a.将环氧基硅烷、氨基烯类化合物加入醇钠溶液中,于60~90℃反应7~10h,将环氧基硅烷与氨基烯类化合物反应后产物与溶剂混合,调节pH使其溶胶-凝胶化,并移入自由基引发剂溶液中,在50~80℃下引发聚合,得到中间体1;
b.将中间体1用老化剂浸泡洗涤,得到中间体2;
c.将中间体2加入硅烷化试剂溶液中静置、冲洗,最后在60~100℃条件下干燥,得到二氧化硅气凝胶。
3.根据权利要求2所述改进的节能环保恒温袋,其特征在于,所述环氧基硅烷的结构为中任一种或多种组合,其中R1、R2、R4、R5独立选自为甲基、甲氧基、乙氧基中任一种,R3、R6各含有环氧基团。
4.根据权利要求2所述改进的节能环保恒温袋,其特征在于,所述环氧基硅烷包括二乙氧基甲基[(3-环氧乙烷基甲氧)丙基]硅烷、3-缩水甘油醚氧基丙基三乙氧基硅烷、3-缩水甘油醚氧基丙基三甲氧基硅烷、(3-环氧丙氧基丙基)二甲基乙氧基硅烷、3-[(2,3)-环氧丙氧]丙基甲基二甲氧基硅烷。
5.根据权利要求2所述改进的节能环保恒温袋,其特征在于,所述氨基烯类化合物包括3-丁烯-1-胺、4-戊烯-1-胺、(E)-丁-2-烯-1-胺、3-甲基-2-丁烯胺、1-氨基-5-己烯。
6.根据权利要求2所述改进的节能环保恒温袋,其特征在于,所述环氧基硅烷、氨基烯类化合物的摩尔比为1:(0.5~1.3)。
7.根据权利要求1所述改进的节能环保恒温袋,其特征在于,所述硫化体系包括硫化剂、促进剂、活性剂、防焦剂。
8.根据权利要求7所述改进的节能环保恒温袋,其特征在于,所述硫化剂、促进剂、活性剂、防焦剂摩尔比为1:(1~1.5):(0.2~0.7):(0.2~0.7)。
9.根据权利要求7~8任一项所述改进的节能环保恒温袋,其特征在于,所述硫化剂为改性高岭土硫化剂。
10.根据权利要求1-9任一项所述改进的节能环保恒温袋制备方法,其特征在于,所述二氧化硅气凝胶表面涂覆胶黏剂,后将二氧化硅气凝胶粘层与橡胶发泡层粘合制备节能环保恒温袋。
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