CN106366242A - 一种电阻型高分子湿敏材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种电阻型高分子湿敏材料，由A、B、C、D四种组分通过聚合反应生成；组分A为丙烯酰氧乙基三甲基氯化铵、甲基丙烯酰丙基三甲基氯化铵、甲基丙烯酰氧乙基三甲基氯化铵中的一种；组分B为N‑甲基烯丙基胺、丙烯酰胺、二甲基烯丙基胺、甲基丙烯酸二甲氨乙酯、甲基丙烯酸二乙氨基乙酯、丙烯酸二甲胺基乙酯中的一种；组分C为甲基丙烯酸甲酯、甲基丙烯酸丁酯、丙烯酸甲酯、丙烯酸丁酯、苯乙烯、烯丙基苯中的一种；组分D为苯乙烯磺酸钠、丙烯酸锂中的一种。本发明的电阻型高分子湿敏材料，其耐高湿性和长期稳定性好。
Description
技术领域
本发明涉及一种高分子材料，具体涉及一种具有湿敏电阻性质的高分子材料及其制备方法。
背景技术
目前商品化的湿度传感器主要有无机陶瓷半导体型和有机高分子型。而高分子型湿度传感器以其响应特性好，测量范围宽，稳定性好，可室温检测，易于集成化，小型化批量生产，价格低廉等优点，已成为湿度传感器的主流。其中，高分子电阻型湿度传感器制备非常简便，性能良好，且易于集成于系统中实现湿度的测量和控制，是湿度传感器研究和发展的之一。然而，这类传感器多采用传统的线型高分子电解质作为敏感材料，它们在高湿环境下容易滑移流失，随着湿度的增加，高分子材料会吸湿膨胀，导致其耐高湿能力和长期稳定性较差，在一定程度上阻碍了其进一步推广应用。为此，需要对高分子湿度敏感材料进行修饰改性，以提高其耐高湿性和长期稳定性。
发明内容
为了克服现有技术的不足，本发明的目的在于提供一种电阻型高分子湿敏材料，其耐高湿性和长期稳定性好。
本发明的另一目的是提供一种所述电阻型高分子湿敏材料的制备方法。
本发明的又一目的是提供由上述电阻型高分子湿敏材料制备而成的湿敏元件。
本发明的目的采用以下技术方案实现：
一种电阻型高分子湿敏材料，所述电阻型高分子湿敏材料由组分A、B、C、D四种组分通过聚合反应生成；
所述组分A为丙烯酰氧乙基三甲基氯化铵、甲基丙烯酰丙基三甲基氯化铵、甲基丙烯酰氧乙基三甲基氯化铵中的一种；
所述组分B为N-甲基烯丙基胺、丙烯酰胺、二甲基烯丙基胺、甲基丙烯酸二甲氨乙酯、甲基丙烯酸二乙氨基乙酯、丙烯酸二甲胺基乙酯中的一种；
所述组分C为甲基丙烯酸甲酯、甲基丙烯酸丁酯、丙烯酸甲酯、丙烯酸丁酯、苯乙烯、烯丙基苯中的一种；
所述组分D为苯乙烯磺酸钠、丙烯酸锂中的一种。
本发明中，聚合反应的机理为：
(1)引发剂偶氮二异丁腈受热，N-N双键断裂，生成自由基
(2)自由基与组分A、B、C、D中的双键发生聚合反应(R1和R2为组分A、B、C、D中与乙烯基相连的基团)
(3)聚合反应持续进行
(4)聚合反应终止，形成电阻型高分子湿敏材料
本发明中优选的方案为，各组分的质量比为A：B：C：D＝1:0.5-2.0:0.5:0.05-0.5。更优选的，各组分的质量比为A:B:C:D＝1:0.5:0.5:0.1。
本发明中优选的方案为，所述组分A为丙烯酰氧乙基三甲基氯化铵，所述组分B为丙烯酰胺，所述组分C为甲基丙烯酸甲酯，所述组分D为丙烯酸锂。
本发明还提供了上述电阻型高分子湿敏材料的制备方法，具体步骤如下：将组分A、B、C、D、引发剂和醇类溶剂加入烧瓶中，在氮气氛围和冷凝回流的条件下，65-85℃恒温反应4-10小时；反应结束后，得到的产物经乙醚洗涤，再于常温下真空干燥，得到电阻型高分子湿敏材料。
本发明中优选的方案为，所述引发剂为偶氮二异丁腈，所述醇类溶剂为甲醇。
本发明中优选的方案为，所述引发剂的添加量为组分A、B、C、D总量的1-5wt％，所述溶剂的添加量为组分A、B、C、D总量的15-30wt％。
本发明还提供了由上述电阻型高分子湿敏材料制备而成的湿敏元件。
本发明中优选的方案为，所述湿敏元件由如下的制备方法制备而成：将电阻型高分子湿敏材料、溶剂和交联剂加入到烧瓶中，在常温下搅拌至电阻型高分子湿敏材料完全溶解，得到湿敏液；再将得到的湿敏液涂敷于叉指电极上，室温放置30-90min，然后在80-110℃下烘烤3-10h，即制得湿敏元件。
本发明中优选的方案为，所述溶剂为N,N-二甲基甲酰胺、N,N-二甲基苯胺、乙醇、异丙醇中的一种，所述交联剂为二溴代烷烃；所述电阻型高分子湿敏材料、溶剂与交联剂的质量比为1:0.5-8:0.05-0.1。
相比现有技术，本发明的有益效果在于：
本发明的电阻型高分子湿敏材料，通过在高分子链中引入疏水性的酯基等链段和可交联性链段，使得高分子材料成膜交联，提高了材料的耐水性，耐高湿性和长期稳定性好；本发明的电阻型高分子湿敏材料，在20-95RH％湿度范围内具有良好的湿度响应，且响应的线性度好，且在整个湿度范围内湿滞小于2RH％。
附图说明
图1为本发明实施例5中的湿敏元件的阻值-湿度关系图；
图2为本发明实施例6中的湿敏元件的阻值-湿度关系图。
具体实施方式
下面，结合附图以及具体实施方式，对本发明做进一步描述：
以下实施方式中，所述“份”为重量份。
以下实施方式中，各组分的CAS号为：丙烯酰氧乙基三甲基氯化铵:44992-01-0；甲基丙烯酰丙基三甲基氯化铵：51410-72-1；甲基丙烯酰氧乙基三甲基氯化铵：5039-78-1；N-甲基烯丙基胺：627-37-2；丙烯酰胺：79-06-1；二甲基烯丙基胺：2155-94-4；甲基丙烯酸二甲氨乙酯：2867-47-2；甲基丙烯酸二乙氨基乙酯：105-16-8；丙烯酸二甲胺基乙酯：2439-35-2；甲基丙烯酸甲酯：80-62-6；甲基丙烯酸丁酯：97-88-1；丙烯酸甲酯：96-33-3；丙烯酸丁酯：141-32-2；苯乙烯：100-42-5；烯丙基苯：300-57-2；苯乙烯磺酸钠：2695-37-6；丙烯酸锂：13270-28-5。
实施例1
取丙烯酰氧乙基三甲基氯化铵20份，丙烯酰胺10份，甲基丙烯酸甲酯10份，丙烯酸锂2份，引发剂AIBN0.5份，置于装有温度计、搅拌器、回流冷凝管和氮气保护装置的四口烧瓶中，加入甲醇，使反应物完全溶解，然后在65-85℃的条件下恒温反应4小时。反应结束后，得到的产物经乙醚洗涤后，于常温真空干燥，得到电阻型高分子湿敏材料。
实施例2
取甲基丙烯酰氧乙基三甲基氯化铵20份，甲基丙烯酸二乙氨基乙酯40份，苯乙烯10份，苯乙烯磺酸钠2份，引发剂AIBN1份，置于装有温度计、搅拌器、回流冷凝管和氮气保护装置的四口烧瓶中，加入甲醇，使反应物完全溶解，然后在65-85℃恒温反应6小时。反应结束后，得到的产物经乙醚洗涤，于常温真空干燥，得到电阻型高分子湿敏材料。
实施例3
取甲基丙烯酰丙基三甲基氯化铵20份，二甲基烯丙基胺20份，丙烯酸甲酯10份，苯乙烯磺酸钠5份，引发剂AIBN0.8份，置于装有温度计、搅拌器、回流冷凝管和氮气保护装置的四口烧瓶中，加入甲醇，使反应物完全溶解，然后在65-85℃恒温反应6小时。反应结束后，得到的产物经乙醚洗涤，于常温真空干燥，得到电阻型高分子湿敏材料。
实施例4
取丙烯酰氧乙基三甲基氯化铵20份，甲基丙烯酸二甲氨乙酯30份，丙烯酸丁酯10份，丙烯酸锂8份，引发剂AIBN1份，置于装有温度计、搅拌器、回流冷凝管和氮气保护装置的四口烧瓶中，加入甲醇，使反应物完全溶解，然后在65-85℃恒温反应6小时。反应结束后，得到的产物经乙醚洗涤，于常温真空干燥，得到电阻型高分子湿敏材料。
实施例5
在装有磁力搅拌子的烧瓶中，依次加入实施例1制备的高分子湿敏材料5份、乙醇20份、1.4-二溴丁烷0.5份，常温磁力搅拌使得原料完全溶解，得到湿敏液；然后将得到的湿敏液涂敷于叉指电极上，室温放置30分钟，然后在80摄氏度下烘烤3个小时，即制得湿敏元件。
实施例6
在装有磁力搅拌子的烧瓶中，依次加入实施例2制备的高分子湿敏材料5份、乙醇20份、1.4-二溴丁烷0.5份，常温磁力搅拌使得原料完全溶解，得到湿敏液。然后将得到的湿敏液涂敷于叉指电极上，室温放置30分钟，然后在80摄氏度下烘烤3个小时，即制得湿敏元件。
性能检测：
分别取实施例5和6制备得到的湿敏元件，置于温湿度标定箱内，从湿度20RH％到95RH％范围内，每隔五个湿度点测试一次材料的阻抗，将获得阻抗数据取对数对湿度值作图，即得到湿敏元件阻值随湿度变化的曲线(见图1和图2)。
从图1和图2中可以看出，本发明的湿敏元件，在20-95RH％的湿度范围内，随着湿度的增加，湿敏元件的阻值呈现下降的趋势，且两者具有良好的线性关系。这表明该湿敏元件具有良好的湿度响应，且响应的线性度好。
对本领域的技术人员来说，可根据以上描述的技术方案以及构思，做出其它各种相应的改变以及形变，而所有的这些改变以及形变都应该属于本发明权利要求的保护范围之内。
Claims (10)
1.一种电阻型高分子湿敏材料，其特征在于，所述电阻型高分子湿敏材料由组分A、B、C、D四种组分通过聚合反应生成；
所述组分A为丙烯酰氧乙基三甲基氯化铵、甲基丙烯酰丙基三甲基氯化铵、甲基丙烯酰氧乙基三甲基氯化铵中的一种；
所述组分B为N-甲基烯丙基胺、丙烯酰胺、二甲基烯丙基胺、甲基丙烯酸二甲氨乙酯、甲基丙烯酸二乙氨基乙酯、丙烯酸二甲胺基乙酯中的一种；
所述组分C为甲基丙烯酸甲酯、甲基丙烯酸丁酯、丙烯酸甲酯、丙烯酸丁酯、苯乙烯、烯丙基苯中的一种；
所述组分D为苯乙烯磺酸钠、丙烯酸锂中的一种。
2.如权利要求1所述的电阻型高分子湿敏材料，其特征在于，各组分的质量比为A：B：C：D＝1:0.5-2.0:0.5:0.05-0.5。
3.如权利要求2所述的电阻型高分子湿敏材料，其特征在于，各组分的质量比为A：B：C：D＝1:0.5:0.5:0.1。
4.如权利要求1所述的电阻型高分子湿敏材料，其特征在于，所述组分A为丙烯酰氧乙基三甲基氯化铵，所述组分B为丙烯酰胺，所述组分C为甲基丙烯酸甲酯，所述组分D为丙烯酸锂。
5.一种如权利要求1-4任一项所述的电阻型高分子湿敏材料的制备方法，其特征在于，将A、B、C、D、引发剂和醇类溶剂加入烧瓶中，在氮气氛围和冷凝回流的条件下，65-85℃恒温反应4-10小时；反应结束后，得到的产物经乙醚洗涤，再于常温下真空干燥，得到电阻型高分子湿敏材料。
6.如权利要求5所述的电阻型高分子湿敏材料的制备方法，其特征在于，所述引发剂为偶氮二异丁腈，所述醇类溶剂为甲醇。
7.如权利要求5所述的电阻型高分子湿敏材料的制备方法，其特征在于，所述引发剂的添加量为组分A、B、C、D总量的1-5wt％，所述溶剂的添加量为组分A、B、C、D总量的15-30wt％。
8.一种由权利要求1-4任一项所述的电阻型高分子湿敏材料制备而成的湿敏元件。
9.如权利要求8所述的湿敏元件，其特征在于，由如下的制备方法制备而成：将电阻型高分子湿敏材料、溶剂和交联剂加入到烧瓶中，在常温下搅拌至电阻型高分子湿敏材料完全溶解，得到湿敏液；再将得到的湿敏液涂敷于叉指电极上，室温放置30-90min，然后在80-110℃下烘烤3-10h，即制得湿敏元件。
10.如权利要求9所述的湿敏元件，其特征在于，所述溶剂为N,N-二甲基甲酰胺、N,N-二甲基苯胺、乙醇、异丙醇中的一种，所述交联剂为二溴代烷烃；所述电阻型高分子湿敏材料、溶剂与交联剂的质量比为1:0.5-8:0.05-0.1。
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4520341A (en) * | 1981-12-08 | 1985-05-28 | Sharp Kabushiki Kaisha | Moisture responsive element with crosslinked organic membrane and protective layering |
| CN105044162A (zh) * | 2015-08-21 | 2015-11-11 | 吉林大学 | 一种高分子基电阻型湿敏元件及其制备方法 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4520341A (en) * | 1981-12-08 | 1985-05-28 | Sharp Kabushiki Kaisha | Moisture responsive element with crosslinked organic membrane and protective layering |
| CN105044162A (zh) * | 2015-08-21 | 2015-11-11 | 吉林大学 | 一种高分子基电阻型湿敏元件及其制备方法 |
Non-Patent Citations (1)
| Title |
|---|
| 陈丽华等: "高分子湿敏器件的修饰改性", 《郑州轻工业学院学报（自然科学版）》 * |
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|---|---|---|---|---|
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