CN116656071A - 一种导热相变水凝胶及其制备方法 - Google Patents
一种导热相变水凝胶及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种导热相变水凝胶,按照质量份数由以下组分制备而成:无机水合盐:20~40份;成核剂:1~5份;增稠剂:1~5份;反应单体:5~15份;交联剂:交联剂为反应单体质量的0.01%~3%;引发剂:引发剂为反应单体质量的0.005%~3.5%;导热填充剂:5~27份;水:40~95份;制得的水凝胶是一种具有三维网状结构,能够将无机水合盐和导热填充剂包封在其中;具有良好的形状稳定性、抗泄露性和导热性能,以及良好的机械性能。
Description
技术领域
本发明涉及一种相变水凝胶,尤其涉及一种导热相变水凝胶,还涉及上述水凝胶的制备方法。
背景技术
太阳能具有来源广泛、无需开采、清洁且对环境友好等优点,是一种应用前景十分广阔的可再生能源,将其高效利用起来可以大大减少人们对化石能源的依赖,对太阳能储热系统进行改进,从而提升光、热资源的利用率是目前发展太阳能热水系统的关键所在。相变材料不仅能量密度较高,而且所用装置简单、使用方便且易于管理,因此,将相变储能技术用于太阳能热水器是当前的研究热点。
相变材料不但能够储存大量的相变潜热,还能够在固体-液体相变过程中维持一定的温度。将相变材料应用到太阳能热水系统中,涉及到材料化学、光热转化和建筑能耗等多个领域的交叉问题。专利CN201510869699.X公开了一种高性能硅基导热凝胶及其制备方法,但其导热系数仅4.2W/(m·K),无法适用于发热量大的应用场景。专利CN201810470129.7公开了一种无硅高K值相变导热凝胶,该凝胶由无硅基体、铂金催化剂、相变蜡、导热填料、交联剂、消泡剂等组成,导热系数也达到了5.5W/(m·K),但由于采用了石蜡、微晶蜡、棕榈蜡,这几种石蜡长期在120℃高温下会出现挥发、分解的问题,同时石蜡、微晶蜡、棕榈蜡存在相变后析出的问题。无机盐水合盐在固-液相变过程中容易泄露和导热性差的问题十分影响材料相变潜热的发挥,石蜡的挥发使其超过其熔点后就失去了相变可逆性。
发明内容
发明目的:本发明的目的在于提供一种无泄露问题、过冷度较低、相变潜热较大、热导率较高且有良好的弹性和形状稳定性的导热相变水凝胶,第二目的在于提供上述导热相变水凝胶的制备方法。
技术方案:本发明的导热相变水凝胶,按质量份数由以下组分制备而成:
无机水合盐:20~40份;
成核剂:1~5份;
增稠剂:1~5份;
反应单体:5~15份;
交联剂:交联剂为反应单体质量的0.01%~3%;
引发剂:引发剂为反应单体质量的0.005%~3.5%;
导热填充剂:5~27份;
水:40~95份。
优选的,所述的无机水合盐为十水硫酸钠、六水氯化钙、十二水磷酸氢二钠、六水氯化镁、十水碳酸钠、四水氯化锌、十水四硼酸钠、四水乙酸镁、六水硝酸镁、四水硝酸钙、九水硝酸铝、六水硝酸锌或三水醋酸钠中的一种。
优选的,所述成核剂为六水氯化锶、八水合氢氧化钡、九水硅酸钠、十水四硼酸钠、六偏磷酸钠、十二水磷酸氢二钠中的一种或多种。
优选的,所述无机水合盐与成核剂之间的晶胞参数差值小于等于15%。
优选的,所述增稠剂为羧甲基纤维素钠、羟乙基纤维素、聚丙烯酰胺、聚丙烯酸钠或羟丙基甲基纤维素中的一种或多种。
优选的,所述反应单体为丙烯酸、甲基丙烯酸、甲基丙烯酸-2-羟乙酯、丙烯酸-2-羟乙酯、甲基丙烯酸羟丙酯、丙烯酰胺、甲基丙烯酰胺或N-异丙基丙烯酰胺中的一种或多种。
优选的,所述交联剂为甲叉双丙烯酰胺或2,2,2-三(丙烯酰氧基)乙醇,所述的引发剂为偶氮类引发剂。
优选的,所述导热填充剂为氧化石墨烯、碳纳米管、MXene纳米片、炭黑、石墨、碳化硅、氮化铝、氮化硼、三氧化二铝或二氧化硅中的一种或多种。
本发明还提供了上述导热相变水凝胶的制备方法,包括以下步骤:
(1)将无机水合盐,成核剂溶解于水中,搅拌均匀得到混合溶液A;
(2)向混合溶液A中加入增稠剂,水浴搅拌均匀得到混合溶液B;
(3)向混合溶液B中加入反应单体、交联剂,搅拌均匀得到混合溶液C;
(4)向混合溶液C中加入导热填充剂,超声分散得到均质混合溶液D;
(5)向混合溶液D中加入引发剂,引发聚合反应,得到导热相变水凝胶。
优选的,步骤(2)中,水浴搅拌的温度为40~60℃。
优选的,步骤(4)中,超声分散的时间为20~50min。
发明原理:本发明的水凝胶相变过程中几乎不存在过冷现象和相分离现象,具有良好的形状稳定性和抗泄露性能,材料在相变前后都能保持很好的固体状态。该水凝胶采用自由基聚合的方式合成,其中无机水合盐和导热填充剂被包封在水凝胶的三维网络结构中,使得该水凝胶具有较高的相变潜热和良好的导热性能,同时,该水凝胶具有良好的形状稳定性能够被制备成各种体积、形状需求的材料。
本发明的水凝胶采用无机水合盐和成核剂协同达到极佳的相变功能,在体系中起到吸收和储存能量的作用,在体系中首先将水合盐粒子溶解于水凝胶前驱体溶液当中,再加入引发剂过硫酸铵引发前驱体溶液中的丙烯酰胺单体发生自由基聚合反应,从而将水合盐粒子封装入聚丙酰胺水凝胶骨架中,制备得到具有相变功能的水凝胶,同时无机水合盐与水凝胶骨架进行结合,解决了无机水合盐易泄露的问题并带来弹性和稳定性,无机水合盐匹配特定成核剂的原则是,两者之间的晶胞参数之差要在15%以内;同时,水凝胶的辅助使水合盐的相变潜热吸收效果大幅上升,可以直接在太阳能吸热领域进行运用,导热填充剂进一步增强了相变水凝胶吸热的效果,未添加导热填充剂的相变水凝胶,仅能吸收外界环境的显热(如贴近一杯热开水直接吸收热量),无法对太阳能进行有效吸收,而填充剂的加入使得相变水凝胶具有了捕获太阳光子的作用,能够吸收紫外和可见光范围以及部分近红外区域光波的能量,增强了相变水凝胶在这些区域的能量吸收效果,使其能够应用于太阳能储能领域。
本发明制备过程中,将导热填充剂超声分散在水凝胶前驱体溶液当中,大大降低了水凝胶在交联过程中能够产生的气泡,同时也提高了水凝胶整体的均匀性。
有益效果:与现有技术相比,本发明具有如下显著优点:(1)本发明的水凝胶具有良好的形状稳定性和抗泄露性能,材料在相变前后都能保持很好的固体状态,同时具有较高的相变潜热和良好的导热性能,导热率最高可达到11.231W/(m·K);(2)制备流程简单,原料来源广泛,价格低廉,具有很好的工业应用前景。
附图说明
图1为本发明实施例1制备得到的导热相变水凝胶的DSC曲线图;
图2为本发明对比例1制备得到的导热相变水凝胶的DSC曲线图;
图3为本发明实施例2制备得到的导热相变水凝胶实物图;
图4为本发明对比例2制备得到的导热相变水凝胶实物图;
图5为本发明实施例1制备得到的导热相变水凝胶实物图。
具体实施方式
下面结合附图和实施例对本发明的技术方案作进一步说明。
实施例1
实施例1的导热相变水凝胶,按质量份数由以下组分制备而成:
六水氯化钙:40g;
六水氯化锶:1.8544g;
羟乙基纤维素:1.9816g;
丙烯酰胺:10.908g;
甲叉双丙烯酰胺:0.1091g;
过硫酸铵:0.0909g;
纳米三氧化二铝:12.726g;
水:72.7g。
实施例1的导热相变水凝胶的制备方法,包括如下步骤:
(1)将40g六水氯化钙,1.8544g六水氯化锶溶解于72.7ml的去离子水中,搅拌均匀得到混合溶液A;
(2)向A溶液中加入1.9816g羟乙基纤维素,并在水浴40℃的条件下加热1h,搅拌均匀得到缓和溶液B;
(3)向混合溶液B中加入10.908g反应单体丙烯酰胺,0.1091g交联剂甲叉双丙烯酰胺,搅拌均匀得到缓和溶液C;
(4)向混合溶液C中加入12.726g的纳米三氧化二铝,超声分散得到均质混合溶液D;
(5)向混合溶液B中加入0.0909g引发剂过硫酸铵,引发聚合反应,得到导热相变水凝胶
实施例1所制备得到的导热相变水凝胶过冷度为0.67℃,相变温度为25.9℃,相变潜热为169.56J/g,热导率为10.4412W/(m·K)。
实施例2
实施例2的导热相变水凝胶,按质量份数由以下组分制备而成:
十水硫酸钠:40g;
十水四硼酸钠:3.009g;
羟乙基纤维素:2.714g;
丙烯酰胺:14.286g;
甲叉双丙烯酰胺:0.2857g;
过硫酸钾:0.2143g;
氮化硼:18.57g;
水:64.48g。
实施例2的导热相变水凝胶的制备方法,包括如下步骤:
(1)将40g十水硫酸钠,3.009g十水四硼酸钠溶解于64.48ml去离子水中,搅拌均匀得到混合溶液A;
(2)向A溶液中加入2.714g羟乙基纤维素,并在水浴40℃的条件下加热1h,搅拌均匀得到缓和溶液B;
(3)向混合溶液B中加入14.286g反应单体丙烯酰胺,0.2857g交联剂甲叉双丙烯酰胺,搅拌均匀得到缓和溶液C;
(4)向混合溶液C中加入18.57g的氮化硼,超声分散得到均质混合溶液D;
(5)向混合溶液B中加入0.2143g引发剂过硫酸钾,引发聚合反应,得到导热相变水凝胶
实施例2所制备得到的导热相变水凝胶为0.32℃,相变温度为32.82℃,相变潜热为122.2087J/g,热导率为9.256W/(m·K)。
实施例3
实施例3的导热相变水凝胶,按质量份数由以下组分制备而成:
十二水磷酸氢二钠:30g;
九水硅酸钠:1.800g;
羧甲基纤维素钠:1.200g;
丙烯酰胺:10g;
2,2,2’-三(丙烯酰氧基)乙醇:0.2000g;
过硫酸钾:0.10g;
氮化硼:12.0g;
水:45g。
实施例3的导热相变水凝胶的制备方法,包括如下步骤:
(1)将30g十二水磷酸氢二钠,1.800g九水硅酸钠溶解于45ml去离子水中,搅拌均匀得到混合溶液A;
(2)向A溶液中加入1.200g羧甲基纤维素钠,并在水浴35℃的条件下加热1h,搅拌均匀得到缓和溶液B;
(3)向混合溶液B中加入10g反应单体丙烯酰胺,0.2000g交联剂2,2,2’-三(丙烯酰氧基)乙醇,搅拌均匀得到缓和溶液C;
(4)向混合溶液C中加入12.0g的氮化硼,超声分散得到均质混合溶液D;
(5)向混合溶液B中加入0.10g引发剂过硫酸钾,引发聚合反应,得到导热相变水凝胶。
实施例3所制备得到的导热相变水凝胶过冷度为1.22℃,相变温度为34.3℃,相变潜热为115.9J/g,热导率为9.231W/(m·K)。
实施例4
实施例4的导热相变水凝胶,按质量份数由以下组分制备而成:
十水硫酸钠:35g;
十水四硼酸钠:2.2400g;
羟乙基纤维素:1.9600;
丙烯酸:11.20g;
甲叉双丙烯酰胺:0.2240g;
过硫酸钾:0.1120g;
纳米氮化铝:15.40g;
水:72.80g。
实施例4的导热相变水凝胶的制备方法,包括如下步骤:
(1)将35g十水硫酸钠,2.2400g十水四硼酸钠溶解于72.80ml去离子水中,搅拌均匀得到混合溶液A;
(2)向A溶液中加入1.9600羟乙基纤维素,并在水浴35℃的条件下加热1h,搅拌均匀得到缓和溶液B;
(3)向混合溶液B中加入11.20g反应单体丙烯酸,0.2240g交联剂甲叉双丙烯酰胺,搅拌均匀得到缓和溶液C;
(4)向混合溶液C中加入15.40g的纳米氮化铝,超声分散得到均质混合溶液D;
(5)向混合溶液B中加入0.1120g引发剂过硫酸钾,引发聚合反应,得到导热相变水凝胶。
实施例4所制备得到的导热相变水凝胶过冷度为1.56℃,相变温度为30.8℃,相变潜热为129.18J/g,热导率为8.796W/(m·K)。
实施例5
实施例5的导热相变水凝胶,按质量份数由以下组分制备而成:
三水醋酸钠:35g;
十二水合磷酸氢二钠:2.800g;
羧甲基纤维素钠:2.4500g;
丙烯酰胺:10.50g;
甲叉双丙烯酰胺:0.2100g;
过硫酸铵:0.1050g;
纳米三氧化二铝:26.25g;
水:91g。
实施例5的导热相变水凝胶的制备方法,包括如下步骤:
(1)将35g三水醋酸钠,2.800g十二水合磷酸氢二钠溶解于91ml去离子水中,搅拌均匀得到混合溶液A;
(2)向A溶液中加入2.4500g羧甲基纤维素钠,并在水浴40℃的条件下加热1h,搅拌均匀得到缓和溶液B;
(3)向混合溶液B中加入10.50g反应单体丙烯酰胺,0.2100g交联剂甲叉双丙烯酰胺,搅拌均匀得到缓和溶液C;
(4)向混合溶液C中加入26.25g的纳米三氧化二铝,超声分散得到均质混合溶液D;
(5)向混合溶液B中加入0.1050g引发剂过硫酸铵,引发聚合反应,得到导热相变水凝胶。
实施例5所制备得到的导热相变水凝胶为0.48℃,相变温度为56.9℃,相变潜热为196.57J/g,热导率为6.286W/(m·K)。
对比例1
与实施例1相比,对比例1制备导热相变水凝胶的步骤中,改变了匹配六水氯化钙的成核剂的种类,
本发明导热相变水凝胶的制备方法,包括如下步骤:
(1)将40g六水氯化钙,1.8544g九水硅酸钠溶解于72.7ml的去离子水中,搅拌均匀得到混合溶液A;
(2)向A溶液中加入1.9816g羟乙基纤维素,并在水浴40℃的条件下加热1h,搅拌均匀得到缓和溶液B;
(3)向混合溶液B中加入10.908g反应单体丙烯酰胺,0.1091g交联剂甲叉双丙烯酰胺,搅拌均匀得到缓和溶液C;
(4)向混合溶液C中加入12.726g的纳米三氧化二铝,超声分散得到均质混合溶液D;
(5)向混合溶液B中加入0.0909g引发剂过硫酸铵,引发聚合反应,得到导热相变水凝胶
对比例1所制备得到的导热相变水凝胶的过冷度为16.6℃,相变温度为26.3℃,相变潜热为75.04J/g,热导率为6.738W/(m·K)。更换了匹配六水氯化钙的成核剂后,相变水凝胶的过冷度变得很大,导致了材料相变潜热的大幅下降。
图1与图2的对比可以看出,不同成核剂对相变潜热的影响极大,更换不匹配六水氯化钙的成核剂后,材料的相变潜热下降了很多,影响相变水凝胶对太阳能的吸收效果。
对比例2
与实施例2相比,对比例2制备导热相变水凝胶的步骤中,改变了无机水合盐十水硫酸钠的用量,具体步骤如下:
(1)将53.20g十水硫酸钠,3.009g十水四硼酸钠溶解于64.48ml去离子水中,搅拌均匀得到混合溶液A;
(2)向A溶液中加入2.714g羟乙基纤维素,并在水浴40℃的条件下加热1h,搅拌均匀得到缓和溶液B;
(3)向混合溶液B中加入14.286g反应单体丙烯酰胺,0.2857g交联剂甲叉双丙烯酰胺,搅拌均匀得到缓和溶液C;
(4)向混合溶液C中加入18.57g的氮化硼,超声分散得到均质混合溶液D;
(5)向混合溶液B中加入0.2143g引发剂过硫酸钾,引发聚合反应,得到导热相变水凝胶
对比例2所制备得到的导热相变水凝胶为14.4℃,相变温度为31.9℃,相变潜热为34.6191J/g,热导率为5.986W/(m·K)。
图3和图4的对比可以看出水合盐份数对材料形貌的影响,水合盐分数超过限定范围后,将导致严重的相分离现象,影响材料相变潜热的发挥,进而影响材料的导热性能。
Claims (10)
1.一种导热相变水凝胶,其特征在于,按质量份数由以下组分制备而成:
无机水合盐:20~40份;
成核剂:1~5份;
增稠剂:1~5份;
反应单体:5~15份;
交联剂:交联剂为反应单体质量的0.01%~3%;
引发剂:引发剂为反应单体质量的0.005%~3.5%;
导热填充剂:5~27份;
水:40~95份。
2.根据权利要求1所述的导热相变水凝胶,其特征在于,所述的无机水合盐为十水硫酸钠、六水氯化钙、十二水磷酸氢二钠、六水氯化镁、十水碳酸钠、四水氯化锌、十水合四硼酸钠、四水乙酸镁、六水硝酸镁、四水硝酸钙、九水硝酸铝、六水硝酸锌或三水醋酸钠中的一种。
3.根据权利要求1所述的导热相变水凝胶,其特征在于,所述成核剂为六水氯化锶、八水合氢氧化钡、九水硅酸钠、十水合四硼酸钠、六偏磷酸钠、十二水磷酸氢二钠中的一种或多种。
4.根据权利要求1所述的导热相变水凝胶,其特征在于,所述无机水合盐与成核剂之间的晶胞参数差值小于等于15%。
5.根据权利要求1所述的导热相变水凝胶,其特征在于,所述反应单体为丙烯酸、甲基丙烯酸、甲基丙烯酸-2-羟乙酯、丙烯酸-2-羟乙酯、甲基丙烯酸羟丙酯、丙烯酰胺、甲基丙烯酰胺或N-异丙基丙烯酰胺中的一种或多种。
6.根据权利要求1所述的导热相变水凝胶,其特征在于,所述增稠剂为羧甲基纤维素钠、羟乙基纤维素、聚丙烯酰胺、聚丙烯酸钠或羟丙基甲基纤维素中的一种或多种,所述交联剂为甲叉双丙烯酰胺或2,2,2-三(丙烯酰氧基)乙醇,所述的引发剂为水溶性氧化物或偶氮类引发剂。
7.根据权利要求1所述的导热相变水凝胶,其特征在于,所述导热填充剂为氧化石墨烯、碳纳米管、MXene纳米片、炭黑、石墨、碳化硅、氮化铝、氮化硼、三氧化二铝或二氧化硅中的一种或多种。
8.一种权利要求1所述的导热相变水凝胶的制备方法,其特征在于,包括以下步骤:
(1)将无机水合盐,成核剂溶解于水中,搅拌均匀得到混合溶液A;
(2)向混合溶液A中加入增稠剂,水浴搅拌均匀得到混合溶液B;
(3)向混合溶液B中加入反应单体、交联剂,搅拌均匀得到混合溶液C;
(4)向混合溶液C中加入导热填充剂,超声分散得到均质混合溶液D;
(5)向混合溶液D中加入引发剂,引发聚合反应,得到导热相变水凝胶。
9.根据权利要求8所述的制备方法,其特征在于,步骤(2)中,水浴搅拌的温度为30~60℃。
10.根据权利要求8所述的制备方法,其特征在于,步骤(4)中,超声分散的时间为20~50min。
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